Revised structures are reported for 30 crystalline compounds, based on space groups of higher symmetry than originally reported. In 18 cases the Laue class is revised, in seven cases the center of symmetry is added, in two cases the Laue class change is coupled with the addition of the center of symmetry, in two cases the addition of the center of symmetry also requires the addition of systematic absences and, finally, one case of the addition of systematic absences without changing the Laue group is reported. Two examples (CSD refcodes: DAMLIM and ABPZCU01) of false polymorphism and one (PAVJUR) of the erroneous interpretation of the fine details of IR spectra, owing to incorrect space-group determination, have been detected.
Supporting information
| Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768104006391/bs0022sup1.cif Contains datablocks global, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 25, 26, 27, 28, 29, 30 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768104006391/bs00222sup2.hkl Contains datablock 2 |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768104006391/bs002212sup3.hkl Contains datablock pajvur |
| Structure factor file (CIF format) https://doi.org/10.1107/S0108768104006391/bs002215sup4.hkl Contains datablock 15 |
| Portable Document Format (PDF) file https://doi.org/10.1107/S0108768104006391/bs0022sup5.pdf Supplementary material |
CCDC references: 241426; 241427; 241428; 241429; 241430; 241431; 241432; 241433; 241434; 241435; 241436; 241437; 241438; 241439; 241440; 241441; 241442; 241443; 241444; 241445; 241446; 241447; 241448; 241449; 241450; 241451; 241452; 241453; 241454
Program(s) used to solve structure: SHELXS97 (Sheldrick, 1990) for (2), (12), (15), (18), (23), (29). Program(s) used to refine structure: SHELXL97 (Sheldrick, 1997) for (2), (12), (15), (18), (23), (29). Software used to prepare material for publication: PLATON (Spek, 1990) for (1), (3), (4), (5), (6), (7), (8), (9), (10), (11), (13), (14), (16), (17), (19), (20), (21), (22), (25), (26), (27), (28), (30).
(1)
cis-Diaqua-(2,2-bipyridyl-N,
N')-copper sulfate
top
Crystal data top
C10H12CuN2O6S | γ = 90° |
Mr = 351.84 | V = 1265.9 (3) Å3 |
Monclinic, I2/a | Z = 4 |
Hall symbol: -I 2ya | F(000) = 668 |
a = 6.963 (1) Å | Dx = 1.783 Mg m−3 |
b = 12.4686 (16) Å | Mo K\a radiation, λ = 0.71070 Å |
c = 14.8540 (15) Å | µ = 1.92 mm−1 |
α = 90° | T = 0 K |
β = 101.01 (1)° | × × mm |
Crystal data top
C10H12CuN2O6S | γ = 90° |
Mr = 351.84 | V = 1265.9 (3) Å3 |
Monclinic, I2/a | Z = 4 |
a = 6.963 (1) Å | Mo K\a radiation |
b = 12.4686 (16) Å | µ = 1.92 mm−1 |
c = 14.8540 (15) Å | T = 0 K |
α = 90° | × × mm |
β = 101.01 (1)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 0.75 | 0.27434 | 0.5 | 0.02* | |
S1 | 0.25 | 0.3461 | 0.5 | 0.02* | |
O1 | 0.42125 | 0.28015 | 0.5348 | 0.02* | |
O2 | 0.20633 | 0.41637 | 0.57487 | 0.02* | |
O5 | 0.653 | 0.38345 | 0.40585 | 0.02* | |
N1 | 0.68405 | 0.1524 | 0.4118 | 0.02* | |
C1 | 0.61755 | 0.16135 | 0.32125 | 0.02* | |
C2 | 0.57847 | 0.07333 | 0.26497 | 0.02* | |
C3 | 0.6068 | −0.02790 | 0.30380 | 0.02* | |
C4 | 0.67475 | −0.03815 | 0.3973 | 0.02* | |
C5 | 0.71223 | 0.05418 | 0.44967 | 0.02* | |
Geometric parameters (Å, º) top
Cu1—O1 | 2.4422 | N1—C5 | 1.3463 |
Cu1—O5 | 1.9754 | C1—C2 | 1.375 |
Cu1—N1 | 2.0023 | C2—C3 | 1.3861 |
S1—O1 | 1.4594 | C3—C4 | 1.385 |
S1—O2 | 1.492 | C4—C5 | 1.386 |
N1—C1 | 1.3409 | C5—C5i | 1.4872 |
| | | |
Cu1···S1ii | 3.5946 (5) | O5···O2iii | 2.6047 |
Cu1···O2ii | 3.6221 | O5···O2vi | 2.6766 |
Cu1···O2iii | 3.6221 | C2···C3vii | 3.4876 |
S1···Cu1iv | 3.5946 (5) | C3···C2viii | 3.4876 |
O1···C4v | 3.2903 | C3···C3vii | 3.5503 |
O2···Cu1iv | 3.6221 | C3···C3viii | 3.5503 |
O2···Cu1iii | 3.6221 | C4···O1v | 3.2903 |
O2···O5iii | 2.6047 | C4···C5vii | 3.4603 |
O2···O5vi | 2.6766 | C5···C4viii | 3.4603 |
| | | |
O1—Cu1—O5 | 85.52 | O1—S1—O1iii | 111.41 |
O1—Cu1—N1 | 93.09 | O1—S1—O2iii | 109.02 |
O1—Cu1—O1i | 176.6 | O1iii—S1—O2 | 109.02 |
O1—Cu1—O5i | 92.14 | O2—S1—O2iii | 108.08 |
O1—Cu1—N1i | 89.49 | O1iii—S1—O2iii | 109.63 |
O5—Cu1—N1 | 93.16 | Cu1—O1—S1 | 132.63 |
O1i—Cu1—O5 | 92.14 | Cu1—N1—C1 | 125.82 |
O5—Cu1—O5i | 92.94 | Cu1—N1—C5 | 114.86 |
O5—Cu1—N1i | 172.26 | C1—N1—C5 | 119.32 |
O1i—Cu1—N1 | 89.49 | N1—C1—C2 | 122.26 |
O5i—Cu1—N1 | 172.26 | C1—C2—C3 | 118.55 |
N1—Cu1—N1i | 81.19 | C2—C3—C4 | 119.7 |
O1i—Cu1—O5i | 85.52 | C3—C4—C5 | 118.54 |
O1i—Cu1—N1i | 93.09 | N1—C5—C4 | 121.62 |
O5i—Cu1—N1i | 93.16 | N1—C5—C5i | 114.54 |
O1—S1—O2 | 109.63 | C4—C5—C5i | 123.83 |
| | | |
O5—Cu1—O1—S1 | −4.09 | Cu1—N1—C1—C2 | 178.95 |
N1—Cu1—O1—S1 | −97.02 | C5—N1—C1—C2 | −0.64 |
O5i—Cu1—O1—S1 | 88.69 | Cu1—N1—C5—C5i | −0.12 |
N1i—Cu1—O1—S1 | −178.17 | C1—N1—C5—C5i | 179.52 |
O1—Cu1—N1—C1 | 91.43 | Cu1—N1—C5—C4 | −179.43 |
O1—Cu1—N1—C5 | −88.96 | C1—N1—C5—C4 | 0.2 |
O5—Cu1—N1—C1 | 5.76 | N1—C1—C2—C3 | 0.82 |
O5—Cu1—N1—C5 | −174.64 | C1—C2—C3—C4 | −0.56 |
O1i—Cu1—N1—C1 | −86.36 | C2—C3—C4—C5 | 0.15 |
O1i—Cu1—N1—C5 | 93.25 | C3—C4—C5—N1 | 0.03 |
N1i—Cu1—N1—C1 | −179.56 | C3—C4—C5—C5i | −179.22 |
N1i—Cu1—N1—C5 | 0.04 | N1—C5—C5i—N1i | 0.15 |
O2—S1—O1—Cu1 | −113.87 | N1—C5—C5i—C4i | 179.45 |
O1iii—S1—O1—Cu1 | 125.38 | C4—C5—C5i—N1i | 179.45 |
O2iii—S1—O1—Cu1 | 4.26 | C4—C5—C5i—C4i | −1.25 |
Symmetry codes: (i) −x+3/2, y, −z+1; (ii) x+1, y, z; (iii) −x+1/2, y, −z+1; (iv) x−1, y, z; (v) −x+1, −y, −z+1; (vi) −x+1, −y+1, −z+1; (vii) x−1/2, −y, z; (viii) x+1/2, −y, z. |
(2) Dinitro-(1,4,7,10-tetra-azacyclododecane) cobalt(iii) chloride monhydrate
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Crystal data top
C8H20CoN6O4·H2O·Cl | Z = 4 |
Mr = 376.70 | F(000) = 784 |
Orthorhombic, Cmc21 | Dx = 1.698 Mg m−3 |
Hall symbol: C 2c -2 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.515 (7) Å | µ = 1.38 mm−1 |
b = 11.909 (9) Å | T = 293 K |
c = 13.003 (10) Å | × × mm |
V = 1473.4 (19) Å3 | |
Data collection top
Radiation source: fine-focus sealed tube | θmax = 25.1°, θmin = 2.7° |
1146 measured reflections | h = −8→11 |
654 independent reflections | k = −8→14 |
652 reflections with I > 2σ(I) | l = −15→0 |
Rint = 0.037 | |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.028 | w = 1/[σ2(Fo2) + (0.P)2 + 3.9018P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.088 | (Δ/σ)max = 0.008 |
S = 1.46 | Δρmax = 0.28 e Å−3 |
654 reflections | Δρmin = −0.32 e Å−3 |
118 parameters | Extinction correction: nne |
2 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.01 (7) |
Secondary atom site location: difference Fourier map | |
Crystal data top
C8H20CoN6O4·H2O·Cl | V = 1473.4 (19) Å3 |
Mr = 376.70 | Z = 4 |
Orthorhombic, Cmc21 | Mo Kα radiation |
a = 9.515 (7) Å | µ = 1.38 mm−1 |
b = 11.909 (9) Å | T = 293 K |
c = 13.003 (10) Å | × × mm |
Data collection top
1146 measured reflections | 652 reflections with I > 2σ(I) |
654 independent reflections | Rint = 0.037 |
Refinement top
R[F2 > 2σ(F2)] = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.088 | Δρmax = 0.28 e Å−3 |
S = 1.46 | Δρmin = −0.32 e Å−3 |
654 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
118 parameters | Absolute structure parameter: −0.01 (7) |
2 restraints | |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is nt relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.5000 | 0.42147 (10) | 0.50007 (13) | 0.0194 (4) | |
O14 | 0.3888 (9) | 0.5481 (7) | 0.6579 (7) | 0.058 (2) | |
O17 | 0.3895 (8) | 0.6053 (6) | 0.4014 (8) | 0.060 (2) | |
N1 | 0.2946 (6) | 0.3988 (4) | 0.4964 (9) | 0.0262 (13) | |
H1 | 0.2514 | 0.4652 | 0.5105 | 0.03 (2)* | |
N4 | 0.5000 | 0.3424 (8) | 0.3680 (7) | 0.022 (2) | |
H6 | 0.5000 | 0.3965 | 0.3187 | 0.04 (4)* | |
N10 | 0.5000 | 0.2873 (8) | 0.5844 (8) | 0.025 (2) | |
H16 | 0.5000 | 0.2265 | 0.5419 | 0.04 (4)* | |
N13 | 0.5000 | 0.5147 (9) | 0.6200 (9) | 0.033 (3) | |
N16 | 0.5000 | 0.5621 (8) | 0.4251 (8) | 0.028 (2) | |
C2 | 0.2552 (10) | 0.3628 (8) | 0.3918 (7) | 0.029 (2) | |
H2 | 0.2513 | 0.4270 | 0.3460 | 0.03 (2)* | |
H3 | 0.1636 | 0.3270 | 0.3926 | 0.04 (3)* | |
C3 | 0.3662 (13) | 0.2805 (9) | 0.3558 (8) | 0.027 (3) | |
H4 | 0.3656 | 0.2131 | 0.3977 | 0.015 (19)* | |
H5 | 0.3511 | 0.2597 | 0.2845 | 0.03 (3)* | |
C8 | 0.2499 (11) | 0.3130 (8) | 0.5755 (7) | 0.035 (2) | |
H12 | 0.1720 | 0.3425 | 0.6152 | 0.04 (3)* | |
H13 | 0.2182 | 0.2455 | 0.5409 | 0.07 (4)* | |
C9 | 0.3691 (15) | 0.2845 (9) | 0.6465 (8) | 0.031 (3) | |
H14 | 0.3744 | 0.3386 | 0.7021 | 0.03 (2)* | |
H15 | 0.3555 | 0.2104 | 0.6759 | 0.03 (2)* | |
O19 | 0.5000 | 0.0551 (14) | 0.2499 (13) | 0.107 (6) | |
H21 | 0.4370 | −0.0102 | 0.1971 | 0.36 (19)* | |
Cl1 | 0.0000 | 0.4637 (2) | 0.0112 (4) | 0.0369 (8) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0240 (6) | 0.0177 (6) | 0.0164 (6) | 0.000 | 0.000 | −0.0002 (8) |
O14 | 0.064 (5) | 0.054 (4) | 0.056 (5) | 0.007 (4) | 0.013 (4) | −0.028 (4) |
O17 | 0.052 (5) | 0.039 (4) | 0.088 (7) | 0.018 (4) | −0.002 (5) | 0.024 (5) |
N1 | 0.026 (3) | 0.026 (3) | 0.027 (3) | 0.004 (2) | 0.004 (5) | 0.001 (5) |
N4 | 0.028 (5) | 0.024 (5) | 0.013 (5) | 0.000 | 0.000 | 0.001 (4) |
N10 | 0.026 (5) | 0.026 (5) | 0.021 (5) | 0.000 | 0.000 | −0.001 (5) |
N13 | 0.046 (7) | 0.024 (6) | 0.028 (6) | 0.000 | 0.000 | −0.005 (5) |
N16 | 0.041 (6) | 0.014 (5) | 0.030 (6) | 0.000 | 0.000 | −0.001 (4) |
C2 | 0.025 (5) | 0.031 (4) | 0.032 (5) | −0.004 (4) | −0.002 (4) | 0.002 (4) |
C3 | 0.026 (6) | 0.031 (6) | 0.026 (5) | 0.000 (5) | −0.007 (5) | −0.004 (4) |
C8 | 0.031 (5) | 0.042 (5) | 0.032 (5) | −0.004 (5) | 0.009 (4) | 0.004 (4) |
C9 | 0.038 (7) | 0.025 (5) | 0.030 (6) | −0.002 (5) | 0.010 (6) | 0.002 (4) |
O19 | 0.165 (16) | 0.083 (10) | 0.072 (10) | 0.000 | 0.000 | −0.008 (9) |
Cl1 | 0.0317 (13) | 0.0274 (12) | 0.052 (2) | 0.000 | 0.000 | −0.0009 (18) |
Geometric parameters (Å, º) top
Co1—N13 | 1.915 (11) | N1—C8 | 1.510 (12) |
Co1—N10 | 1.938 (10) | N4—C3 | 1.479 (13) |
Co1—N16 | 1.938 (10) | N4—C3i | 1.479 (13) |
Co1—N4 | 1.958 (9) | N10—C9i | 1.485 (13) |
Co1—N1 | 1.974 (6) | N10—C9 | 1.485 (13) |
Co1—N1i | 1.974 (6) | N13—O14i | 1.233 (9) |
O14—N13 | 1.233 (9) | N16—O17i | 1.211 (8) |
O17—N16 | 1.211 (8) | C2—C3 | 1.515 (15) |
N1—C2 | 1.474 (14) | C8—C9 | 1.501 (17) |
| | | |
N13—Co1—N10 | 91.0 (5) | C8—N1—Co1 | 110.8 (6) |
N13—Co1—N16 | 84.8 (5) | C3—N4—C3i | 118.7 (10) |
N10—Co1—N16 | 175.7 (5) | C3—N4—Co1 | 109.5 (6) |
N13—Co1—N4 | 173.3 (5) | C3i—N4—Co1 | 109.5 (6) |
N10—Co1—N4 | 95.7 (5) | C9i—N10—C9 | 114.0 (12) |
N16—Co1—N4 | 88.6 (4) | C9i—N10—Co1 | 109.0 (6) |
N13—Co1—N1 | 95.7 (3) | C9—N10—Co1 | 109.0 (6) |
N10—Co1—N1 | 84.3 (2) | O14i—N13—O14 | 118.2 (11) |
N16—Co1—N1 | 96.1 (2) | O14i—N13—Co1 | 120.8 (6) |
N4—Co1—N1 | 85.0 (3) | O14—N13—Co1 | 120.8 (6) |
N13—Co1—N1i | 95.7 (3) | O17i—N16—O17 | 120.6 (11) |
N10—Co1—N1i | 84.3 (2) | O17i—N16—Co1 | 119.7 (5) |
N16—Co1—N1i | 96.1 (2) | O17—N16—Co1 | 119.7 (5) |
N4—Co1—N1i | 85.0 (3) | N1—C2—C3 | 107.2 (8) |
N1—Co1—N1i | 164.0 (3) | N4—C3—C2 | 104.2 (8) |
C2—N1—C8 | 111.1 (7) | C9—C8—N1 | 111.1 (8) |
C2—N1—Co1 | 108.3 (6) | N10—C9—C8 | 107.1 (8) |
| | | |
N13—Co1—N1—C2 | 160.2 (6) | N10—Co1—N13—O14i | 92.1 (9) |
N10—Co1—N1—C2 | −109.3 (6) | N16—Co1—N13—O14i | −87.9 (9) |
N16—Co1—N1—C2 | 74.9 (6) | N1—Co1—N13—O14i | 176.5 (9) |
N4—Co1—N1—C2 | −13.1 (5) | N1i—Co1—N13—O14i | 7.7 (10) |
N1i—Co1—N1—C2 | −65 (3) | N10—Co1—N13—O14 | −92.1 (9) |
N13—Co1—N1—C8 | −77.7 (7) | N16—Co1—N13—O14 | 87.9 (9) |
N10—Co1—N1—C8 | 12.7 (7) | N1—Co1—N13—O14 | −7.7 (10) |
N16—Co1—N1—C8 | −163.0 (7) | N1i—Co1—N13—O14 | −176.5 (9) |
N4—Co1—N1—C8 | 108.9 (7) | N13—Co1—N16—O17i | 90.4 (10) |
N1i—Co1—N1—C8 | 57 (3) | N4—Co1—N16—O17i | −89.6 (10) |
N10—Co1—N4—C3 | 65.9 (6) | N1—Co1—N16—O17i | −174.4 (10) |
N16—Co1—N4—C3 | −114.1 (6) | N1i—Co1—N16—O17i | −4.8 (10) |
N1—Co1—N4—C3 | −17.9 (6) | N13—Co1—N16—O17 | −90.4 (10) |
N1i—Co1—N4—C3 | 149.6 (7) | N4—Co1—N16—O17 | 89.6 (10) |
N10—Co1—N4—C3i | −65.9 (6) | N1—Co1—N16—O17 | 4.8 (10) |
N16—Co1—N4—C3i | 114.1 (6) | N1i—Co1—N16—O17 | 174.4 (10) |
N1—Co1—N4—C3i | −149.6 (7) | C8—N1—C2—C3 | −81.1 (8) |
N1i—Co1—N4—C3i | 17.9 (6) | Co1—N1—C2—C3 | 40.7 (8) |
N13—Co1—N10—C9i | −62.5 (7) | C3i—N4—C3—C2 | 170.1 (7) |
N4—Co1—N10—C9i | 117.5 (7) | Co1—N4—C3—C2 | 43.4 (9) |
N1—Co1—N10—C9i | −158.1 (8) | N1—C2—C3—N4 | −54.7 (10) |
N1i—Co1—N10—C9i | 33.1 (7) | C2—N1—C8—C9 | 130.3 (8) |
N13—Co1—N10—C9 | 62.5 (7) | Co1—N1—C8—C9 | 10.0 (10) |
N4—Co1—N10—C9 | −117.5 (7) | C9i—N10—C9—C8 | 167.9 (6) |
N1—Co1—N10—C9 | −33.1 (7) | Co1—N10—C9—C8 | 45.7 (10) |
N1i—Co1—N10—C9 | 158.1 (8) | N1—C8—C9—N10 | −35.4 (11) |
Symmetry code: (i) −x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O14 | 0.91 | 2.52 | 2.8941 | 105 |
N1—H1···O17 | 0.91 | 2.55 | 2.8964 | 103 |
N1—H1···Cl1ii | 0.91 | 2.54 | 3.2518 | 136 |
N1—H1···Cl1iii | 0.91 | 2.54 | 3.2518 | 136 |
N4—H6···O14iv | 0.91 | 2.43 | 3.2068 | 143 |
N4—H6···O14v | 0.91 | 2.43 | 3.2068 | 143 |
N10—H16···Cl1vi | 0.91 | 2.3 | 3.137 (2) | 153 |
N10—H16···Cl1vii | 0.91 | 2.3 | 3.137 (2) | 153 |
O19—H21···Cl1viii | 1.2 | 2.51 | 3.290 (3) | 121 |
O19—H21···Cl1ix | 1.2 | 2.51 | 3.290 (3) | 121 |
C2—H2···O17 | 0.97 | 2.6 | 3.1609 | 117 |
C9—H14···O14 | 0.97 | 2.56 | 3.1488 | 119 |
Symmetry codes: (ii) −x, −y+1, z+1/2; (iii) x, −y+1, z+1/2; (iv) −x+1, −y+1, z−1/2; (v) x, −y+1, z−1/2; (vi) −x+1/2, −y+1/2, z+1/2; (vii) x+1/2, −y+1/2, z+1/2; (viii) x+1/2, y−1/2, z; (ix) −x+1/2, y−1/2, z. |
(3) 3',6'-
O-(1,1,3,3-Tetraisopropyl-disiloxane-1,3-diyl)-neplancin A
top
Crystal data top
C23H39N5O4Si2 | Z = 8 |
Mr = 505.77 | F(000) = 1864 |
Orthorhombic, C2221 | Dx = 1.119 Mg m−3 |
Hall symbol: C 2c 2 | Mo K\a radiation, λ = 0.71073 Å |
a = 13.1422 (15) Å | µ = 0.16 mm−1 |
b = 12.1676 (15) Å | T = 0 K |
c = 34.638 (4) Å | × × mm |
V = 5538.9 (11) Å3 | |
Refinement top
0 restraints | |
See text | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
Crystal data top
C23H39N5O4Si2 | V = 5538.9 (11) Å3 |
Mr = 505.77 | Z = 8 |
Orthorhombic, C2221 | Mo K\a radiation |
a = 13.1422 (15) Å | µ = 0.16 mm−1 |
b = 12.1676 (15) Å | T = 0 K |
c = 34.638 (4) Å | × × mm |
Refinement top
0 restraints | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
See text | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Si1 | 0.63508 | 0.44078 | 0.13178 | 0.02* | |
Si2 | 0.70738 | 0.66313 | 0.17120 | 0.02* | |
O1 | 0.87493 | 0.27752 | 0.08375 | 0.02* | |
O2 | 0.72665 | 0.43305 | 0.09945 | 0.02* | |
O3 | 0.80542 | 0.68708 | 0.14310 | 0.02* | |
O4 | 0.65175 | 0.5497 | 0.1582 | 0.02* | |
N1 | 1.24808 | 0.24653 | −0.01385 | 0.02* | |
N2 | 1.0726 | 0.2819 | 0.00225 | 0.02* | |
N3 | 1.38228 | 0.34722 | 0.01235 | 0.02* | |
N4 | 1.22315 | 0.47465 | 0.05575 | 0.02* | |
N5 | 1.05572 | 0.43607 | 0.0471 | 0.02* | |
C1 | 1.14848 | 0.22882 | −0.01560 | 0.02* | |
C2 | 1.10867 | 0.36258 | 0.025 | 0.02* | |
C3 | 1.21035 | 0.3877 | 0.0304 | 0.02* | |
C4 | 1.28172 | 0.32783 | 0.00975 | 0.02* | |
C5 | 1.12843 | 0.50022 | 0.0646 | 0.02* | |
C6 | 0.94517 | 0.44578 | 0.05285 | 0.02* | |
C7 | 0.90843 | 0.38718 | 0.0895 | 0.02* | |
C8 | 0.82915 | 0.4653 | 0.10785 | 0.02* | |
C9 | 0.85185 | 0.57315 | 0.08925 | 0.02* | |
C10 | 0.914 | 0.56355 | 0.0595 | 0.02* | |
C11 | 0.80115 | 0.67760 | 0.10205 | 0.02* | |
C12 | 0.65413 | 0.88858 | 0.17395 | 0.02* | |
C13 | 0.61203 | 0.77697 | 0.16485 | 0.02* | |
C14 | 0.5119 | 0.759 | 0.1856 | 0.02* | |
C15 | 0.68975 | 0.62575 | 0.2515 | 0.02* | |
C16 | 0.76565 | 0.6495 | 0.2199 | 0.02* | |
C17 | 0.8508 | 0.5657 | 0.2201 | 0.02* | |
C18 | 0.42198 | 0.46662 | 0.1286 | 0.02* | |
C19 | 0.51508 | 0.45342 | 0.10325 | 0.02* | |
C20 | 0.52295 | 0.5462 | 0.0736 | 0.02* | |
C21 | 0.63133 | 0.21132 | 0.14165 | 0.02* | |
C22 | 0.64267 | 0.31877 | 0.16435 | 0.02* | |
C23 | 0.57 | 0.323 | 0.19905 | 0.02* | |
Geometric parameters (Å, º) top
Si1—O2 | 1.6466 | N5—C5 | 1.3747 |
Si1—O4 | 1.6254 | N5—C6 | 1.4712 |
Si1—C19 | 1.8674 | C2—C3 | 1.3835 |
Si1—C22 | 1.8673 | C3—C4 | 1.3864 |
Si2—O3 | 1.6409 | C6—C7 | 1.534 |
Si2—O4 | 1.6255 | C6—C10 | 1.5081 |
Si2—C13 | 1.8808 | C7—C8 | 1.547 |
Si2—C16 | 1.86 | C8—C9 | 1.492 |
O1—C7 | 1.4191 | C9—C10 | 1.3201 |
O2—C8 | 1.4329 | C9—C11 | 1.5019 |
O3—C11 | 1.4277 | C12—C13 | 1.4999 |
N1—C1 | 1.328 | C13—C14 | 1.5153 |
N1—C4 | 1.3573 | C15—C16 | 1.5088 |
N2—C1 | 1.3394 | C16—C17 | 1.5139 |
N2—C2 | 1.3451 | C18—C19 | 1.5145 |
N3—C4 | 1.3455 | C19—C20 | 1.5297 |
N4—C3 | 1.3851 | C21—C22 | 1.5329 |
N4—C5 | 1.3192 | C22—C23 | 1.536 |
N5—C2 | 1.3674 | | |
| | | |
Si1···C11 | 3.7586 | N4···C4iii | 3.3935 |
Si2···C8 | 3.6291 | C2···C5iii | 3.5336 |
O1···O2 | 2.7703 | C3···N4iii | 3.4261 |
O1···N1i | 2.9542 | C3···C3iii | 3.4502 |
O2···O1 | 2.7703 | C4···N4iii | 3.3935 |
N1···O1ii | 2.9542 | C5···C2iii | 3.5336 |
N2···N3i | 2.9967 | C8···Si2 | 3.6291 |
N3···N4 | 3.0063 | C11···Si1 | 3.7586 |
N3···N2ii | 2.9967 | C18···C23 | 3.5767 |
N4···N3 | 3.0063 | C23···C18 | 3.5767 |
N4···C3iii | 3.4261 | | |
| | | |
O2—Si1—O4 | 109.33 | N1—C4—C3 | 118.25 |
O2—Si1—C19 | 105.19 | N3—C4—C3 | 122.54 |
O2—Si1—C22 | 109.05 | N4—C5—N5 | 114.81 |
O4—Si1—C19 | 110.16 | N5—C6—C7 | 112.68 |
O4—Si1—C22 | 107.51 | N5—C6—C10 | 111.42 |
C19—Si1—C22 | 115.49 | C7—C6—C10 | 103.28 |
O3—Si2—O4 | 109.86 | O1—C7—C6 | 114.74 |
O3—Si2—C13 | 108.85 | O1—C7—C8 | 115.24 |
O3—Si2—C16 | 103.33 | C6—C7—C8 | 105.45 |
O4—Si2—C13 | 107.05 | O2—C8—C7 | 112.43 |
O4—Si2—C16 | 111.14 | O2—C8—C9 | 109.95 |
C13—Si2—C16 | 116.49 | C7—C8—C9 | 103.2 |
Si1—O2—C8 | 122.23 | C8—C9—C10 | 112.52 |
Si2—O3—C11 | 123.06 | C8—C9—C11 | 121.88 |
Si1—O4—Si2 | 155.36 | C10—C9—C11 | 125.44 |
C1—N1—C4 | 117.83 | C6—C10—C9 | 111.8 |
C1—N2—C2 | 111.1 | O3—C11—C9 | 110.18 |
C3—N4—C5 | 102.29 | Si2—C13—C12 | 113.36 |
C2—N5—C5 | 105.33 | Si2—C13—C14 | 114.64 |
C2—N5—C6 | 129.11 | C12—C13—C14 | 110.57 |
C5—N5—C6 | 125.53 | Si2—C16—C15 | 113.75 |
N1—C1—N2 | 129.39 | Si2—C16—C17 | 111.63 |
N2—C2—N5 | 128.74 | C15—C16—C17 | 110.88 |
N2—C2—C3 | 125.51 | Si1—C19—C18 | 112.59 |
N5—C2—C3 | 105.75 | Si1—C19—C20 | 111.04 |
N4—C3—C2 | 111.82 | C18—C19—C20 | 111.45 |
N4—C3—C4 | 130.26 | Si1—C22—C21 | 111.28 |
C2—C3—C4 | 117.88 | Si1—C22—C23 | 114.39 |
N1—C4—N3 | 119.21 | C21—C22—C23 | 111.68 |
| | | |
O4—Si1—O2—C8 | 36.6 | C2—N2—C1—N1 | −0.87 |
C19—Si1—O2—C8 | 154.87 | C1—N2—C2—C3 | −1.26 |
C22—Si1—O2—C8 | −80.69 | C1—N2—C2—N5 | 178.43 |
O2—Si1—C22—C23 | 172.61 | C3—N4—C5—N5 | 0.37 |
O4—Si1—C22—C23 | 54.18 | C5—N4—C3—C2 | −0.63 |
C19—Si1—C22—C23 | −69.24 | C5—N4—C3—C4 | 177.04 |
O2—Si1—O4—Si2 | 3.65 | C5—N5—C6—C7 | −81.86 |
C19—Si1—O4—Si2 | −111.47 | C5—N5—C2—N2 | 179.86 |
C22—Si1—O4—Si2 | 121.91 | C6—N5—C2—C3 | −178.70 |
O2—Si1—C19—C18 | −177.48 | C2—N5—C6—C10 | −148.32 |
O4—Si1—C19—C18 | −59.77 | C5—N5—C2—C3 | −0.40 |
C22—Si1—C19—C18 | 62.24 | C6—N5—C2—N2 | 1.57 |
O2—Si1—C19—C20 | −51.73 | C2—N5—C6—C7 | 96.12 |
O4—Si1—C19—C20 | 65.99 | C6—N5—C5—N4 | 178.39 |
C22—Si1—C19—C20 | −172.00 | C2—N5—C5—N4 | 0.03 |
O2—Si1—C22—C21 | −59.65 | C5—N5—C6—C10 | 33.69 |
O4—Si1—C22—C21 | −178.08 | N5—C2—C3—C4 | −177.32 |
C19—Si1—C22—C21 | 58.5 | N2—C2—C3—N4 | −179.59 |
O4—Si2—O3—C11 | 46.01 | N2—C2—C3—C4 | 2.42 |
C13—Si2—O3—C11 | −70.91 | N5—C2—C3—N4 | 0.67 |
C16—Si2—O3—C11 | 164.67 | N4—C3—C4—N3 | 1.12 |
O4—Si2—C16—C15 | −61.73 | C2—C3—C4—N3 | 178.67 |
C13—Si2—C16—C15 | 61.23 | N4—C3—C4—N1 | −179.04 |
O3—Si2—C16—C17 | −53.11 | C2—C3—C4—N1 | −1.49 |
O4—Si2—C16—C17 | 64.66 | N5—C6—C7—O1 | −93.45 |
C13—Si2—C16—C17 | −172.38 | N5—C6—C7—C8 | 138.63 |
O3—Si2—O4—Si1 | −1.47 | C10—C6—C7—C8 | 18.27 |
C13—Si2—O4—Si1 | 116.57 | N5—C6—C10—C9 | −132.88 |
C16—Si2—O4—Si1 | −115.20 | C10—C6—C7—O1 | 146.19 |
O3—Si2—C13—C12 | −58.51 | C7—C6—C10—C9 | −11.67 |
O4—Si2—C13—C12 | −177.20 | O1—C7—C8—O2 | −27.70 |
C16—Si2—C13—C12 | 57.74 | O1—C7—C8—C9 | −146.11 |
O3—Si2—C13—C14 | 173.24 | C6—C7—C8—O2 | 99.92 |
O4—Si2—C13—C14 | 54.55 | C6—C7—C8—C9 | −18.49 |
C16—Si2—C13—C14 | −70.51 | C7—C8—C9—C11 | −172.38 |
O3—Si2—C16—C15 | −179.50 | O2—C8—C9—C11 | 67.5 |
Si1—O2—C8—C9 | −105.14 | C7—C8—C9—C10 | 12.13 |
Si1—O2—C8—C7 | 140.5 | O2—C8—C9—C10 | −108.00 |
Si2—O3—C11—C9 | −103.60 | C8—C9—C10—C6 | −0.37 |
C4—N1—C1—N2 | 1.67 | C11—C9—C10—C6 | −175.67 |
C1—N1—C4—N3 | 179.53 | C8—C9—C11—O3 | 48.01 |
C1—N1—C4—C3 | −0.32 | C10—C9—C11—O3 | −137.11 |
Symmetry codes: (i) x−1/2, −y+1/2, −z; (ii) x+1/2, −y+1/2, −z; (iii) x, −y+1, −z. |
(4) (
R*,
R*)-4,4'-Bi(1 − t-butylcyclohexen-3-one)
top
Crystal data top
C20H30O2 | γ = 90° |
Mr = 302.44 | V = 1890.5 (13) Å3 |
Monclinic, I2/a | Z = 4 |
Hall symbol: -I 2ya | F(000) = 544 |
a = 27.869 (1) Å | Dx = 0.956 Mg m−3 |
b = 5.771 (3) Å | Mo K\a radiation, λ = 0.71070 Å |
c = 11.758 (5) Å | µ = 0.06 mm−1 |
α = 90° | T = 0 K |
β = 91.43 (1)° | × × mm |
Crystal data top
C20H30O2 | γ = 90° |
Mr = 302.44 | V = 1890.5 (13) Å3 |
Monclinic, I2/a | Z = 4 |
a = 27.869 (1) Å | Mo K\a radiation |
b = 5.771 (3) Å | µ = 0.06 mm−1 |
c = 11.758 (5) Å | T = 0 K |
α = 90° | × × mm |
β = 91.43 (1)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
O1 | 0.18350 | 0.3012 | 0.6195 | 0.02* | |
C1 | 0.2271 | 0.4399 | 0.46215 | 0.02* | |
C2 | 0.22095 | 0.6572 | 0.3911 | 0.02* | |
C3 | 0.17722 | 0.63838 | 0.31233 | 0.02* | |
C4 | 0.13318 | 0.58117 | 0.37758 | 0.02* | |
C5 | 0.13745 | 0.47505 | 0.476 | 0.02* | |
C6 | 0.18245 | 0.39965 | 0.52725 | 0.02* | |
C13 | 0.0849 | 0.65935 | 0.32365 | 0.02* | |
C14 | 0.0423 | 0.5737 | 0.38965 | 0.02* | |
C15 | 0.07998 | 0.57582 | 0.20208 | 0.02* | |
C16 | 0.08325 | 0.9236 | 0.32655 | 0.02* | |
Geometric parameters (Å, º) top
O1—C6 | 1.2242 | C4—C5 | 1.3121 |
C1—C2 | 1.5142 | C4—C13 | 1.5406 |
C1—C6 | 1.4953 | C5—C6 | 1.4448 |
C1—C1i | 1.5378 | C13—C14 | 1.5172 |
C2—C3 | 1.5161 | C13—C15 | 1.5115 |
C3—C4 | 1.5003 | C13—C16 | 1.5261 |
| | | |
O1···C2i | 3.3681 | C2···O1i | 3.3681 |
O1···C3ii | 3.4098 | C3···O1iii | 3.4098 |
| | | |
C2—C1—C6 | 109.08 | O1—C6—C1 | 121.59 |
C1i—C1—C2 | 113.59 | O1—C6—C5 | 120.71 |
C1i—C1—C6 | 113.14 | C1—C6—C5 | 117.68 |
C1—C2—C3 | 110.85 | C4—C13—C14 | 112.37 |
C2—C3—C4 | 111.02 | C4—C13—C15 | 110.7 |
C3—C4—C5 | 119.76 | C4—C13—C16 | 108.06 |
C3—C4—C13 | 116.25 | C14—C13—C15 | 109.03 |
C5—C4—C13 | 123.97 | C14—C13—C16 | 106.84 |
C4—C5—C6 | 124.55 | C15—C13—C16 | 109.74 |
| | | |
C6—C1—C2—C3 | −56.98 | C2—C3—C4—C13 | 153.97 |
C1i—C1—C2—C3 | 175.8 | C3—C4—C5—C6 | −2.00 |
C2—C1—C6—O1 | −150.68 | C13—C4—C5—C6 | 179.63 |
C2—C1—C6—C5 | 31.12 | C3—C4—C13—C14 | 174.42 |
C1i—C1—C6—O1 | −23.20 | C3—C4—C13—C15 | 52.24 |
C1i—C1—C6—C5 | 158.59 | C3—C4—C13—C16 | −67.95 |
C2—C1—C1i—C2i | 50.69 | C5—C4—C13—C14 | −7.16 |
C2—C1—C1i—C6i | −74.38 | C5—C4—C13—C15 | −129.34 |
C6—C1—C1i—C2i | −74.38 | C5—C4—C13—C16 | 110.46 |
C6—C1—C1i—C6i | 160.55 | C4—C5—C6—O1 | −179.90 |
C1—C2—C3—C4 | 54.28 | C4—C5—C6—C1 | −1.67 |
C2—C3—C4—C5 | −24.51 | | |
Symmetry codes: (i) −x+1/2, y, −z+1; (ii) x, −y+1/2, z+1/2; (iii) x, −y+1/2, z−1/2. |
(5)
N-(3-Aminpropyl)-
N'-3-(anthracen-9-ylmethyl)aminpropylethane-1,2-diamin)- chloro-copper chloride monhydrate
top
Crystal data top
C23H32ClCuN4+·Cl−·H2O | γ = 90° |
Mr = 514.98 | V = 4994.3 (12) Å3 |
Monclinic, I2/a | Z = 8 |
Hall symbol: -I 2ya | F(000) = 2152 |
a = 18.6300 (18) Å | Dx = 1.370 Mg m−3 |
b = 16.610 (2) Å | Mo K\a radiation, λ = 0.71070 Å |
c = 16.972 (3) Å | µ = 1.11 mm−1 |
α = 90° | T = 0 K |
β = 108.020 (9)° | × × mm |
Crystal data top
C23H32ClCuN4+·Cl−·H2O | γ = 90° |
Mr = 514.98 | V = 4994.3 (12) Å3 |
Monclinic, I2/a | Z = 8 |
a = 18.6300 (18) Å | Mo K\a radiation |
b = 16.610 (2) Å | µ = 1.11 mm−1 |
c = 16.972 (3) Å | T = 0 K |
α = 90° | × × mm |
β = 108.020 (9)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cu1 | 0.38685 | 0.00029 | 0.3132 | 0.02* | |
Cl1 | 0.4667 | −0.09995 | 0.42675 | 0.02* | |
N1 | 0.47375 | 0.006 | 0.2644 | 0.02* | |
N2 | 0.4234 | 0.1008 | 0.38235 | 0.02* | |
N3 | 0.2944 | 0.00885 | 0.3551 | 0.02* | |
N4 | 0.33455 | −0.09005 | 0.23245 | 0.02* | |
C1 | 0.5107 | 0.0842 | 0.2543 | 0.02* | |
C2 | 0.53215 | 0.1337 | 0.33425 | 0.02* | |
C3 | 0.46522 | 0.16422 | 0.35618 | 0.02* | |
C4 | 0.35667 | 0.13412 | 0.40293 | 0.02* | |
C5 | 0.31337 | 0.06482 | 0.42408 | 0.02* | |
C6 | 0.26297 | −0.06693 | 0.37653 | 0.02* | |
C7 | 0.23575 | −0.12215 | 0.30035 | 0.02* | |
C8 | 0.29708 | −0.15277 | 0.26978 | 0.02* | |
C9 | 0.281 | −0.06250 | 0.1523 | 0.02* | |
C10 | 0.3216 | −0.02465 | 0.0967 | 0.02* | |
C11 | 0.35395 | −0.07415 | 0.04835 | 0.02* | |
C12 | 0.34935 | −0.16110 | 0.04835 | 0.02* | |
C13 | 0.379 | −0.20570 | −0.00205 | 0.02* | |
C14 | 0.4122 | −0.16955 | −0.05620 | 0.02* | |
C15 | 0.41832 | −0.08777 | −0.05823 | 0.02* | |
C16 | 0.38878 | −0.03863 | −0.00738 | 0.02* | |
C17 | 0.39452 | 0.04557 | −0.00993 | 0.02* | |
C18 | 0.36705 | 0.0939 | 0.04040 | 0.02* | |
C19 | 0.3774 | 0.1786 | 0.0405 | 0.02* | |
C20 | 0.35137 | 0.22688 | 0.08968 | 0.02* | |
C21 | 0.31125 | 0.194 | 0.1406 | 0.02* | |
C22 | 0.3001 | 0.11275 | 0.1434 | 0.02* | |
C23 | 0.32825 | 0.05915 | 0.0942 | 0.02* | |
Cl3 | 0.13337 | 0.09933 | 0.24243 | 0.02* | |
O1 | 0.52355 | 0.31205 | 0.2397 | 0.02* | |
H1 | 0.45685 | −0.01670 | 0.21385 | 0.02* | |
H2 | 0.51118 | −0.02602 | 0.29547 | 0.02* | |
H3 | 0.45572 | 0.08272 | 0.43132 | 0.02* | |
H4 | 0.25625 | 0.0321 | 0.3137 | 0.02* | |
H5 | 0.37305 | −0.11590 | 0.2195 | 0.02* | |
H6 | 0.5564 | 0.07345 | 0.2389 | 0.02* | |
H7 | 0.47565 | 0.115 | 0.21 | 0.02* | |
H8 | 0.56333 | 0.17902 | 0.32828 | 0.02* | |
H9 | 0.56297 | 0.10057 | 0.37938 | 0.02* | |
H10 | 0.4309 | 0.19155 | 0.3085 | 0.02* | |
H11 | 0.48255 | 0.2033 | 0.4005 | 0.02* | |
H12 | 0.37378 | 0.17063 | 0.44963 | 0.02* | |
H13 | 0.32387 | 0.16367 | 0.35598 | 0.02* | |
H14 | 0.26695 | 0.0842 | 0.43365 | 0.02* | |
H15 | 0.34458 | 0.03833 | 0.47402 | 0.02* | |
H16 | 0.30207 | −0.09427 | 0.42018 | 0.02* | |
H17 | 0.2203 | −0.05500 | 0.39695 | 0.02* | |
H18 | 0.19940 | −0.09275 | 0.25595 | 0.02* | |
H19 | 0.20888 | −0.16768 | 0.31413 | 0.02* | |
H20 | 0.33582 | −0.17797 | 0.31543 | 0.02* | |
H21 | 0.27595 | −0.19400 | 0.2285 | 0.02* | |
H22 | 0.25128 | −0.10812 | 0.12393 | 0.02* | |
H23 | 0.24567 | −0.02367 | 0.16287 | 0.02* | |
H24 | 0.32605 | −0.18680 | 0.08295 | 0.02* | |
H25 | 0.37690 | −0.26160 | 0 | 0.02* | |
H26 | 0.43035 | −0.20120 | −0.09130 | 0.02* | |
H27 | 0.4422 | −0.06410 | −0.09340 | 0.02* | |
H28 | 0.41727 | 0.06912 | −0.04618 | 0.02* | |
H29 | 0.40258 | 0.20122 | 0.00602 | 0.02* | |
H30 | 0.35995 | 0.28205 | 0.09 | 0.02* | |
H31 | 0.29205 | 0.2281 | 0.17290 | 0.02* | |
H32 | 0.27375 | 0.09235 | 0.17785 | 0.02* | |
Geometric parameters (Å, º) top
Cu1—Cl1 | 2.6316 | C18—C19 | 1.4199 |
Cu1—N1 | 2.0361 | C18—C23 | 1.4484 |
Cu1—N2 | 2.0332 | C19—C20 | 1.3511 |
Cu1—N3 | 2.0616 | C20—C21 | 1.4154 |
Cu1—N4 | 2.0623 | C21—C22 | 1.3685 |
N1—C1 | 1.5045 | C22—C23 | 1.4268 |
N2—C3 | 1.4588 | C1—H6 | 0.9812 |
N2—C4 | 1.4975 | C1—H7 | 0.9745 |
N3—C5 | 1.4504 | C2—H8 | 0.9751 |
N3—C6 | 1.4803 | C2—H9 | 0.9732 |
N4—C8 | 1.4992 | C3—H10 | 0.9745 |
N4—C9 | 1.4884 | C3—H11 | 0.9701 |
N1—H1 | 0.9001 | C4—H12 | 0.9702 |
N1—H2 | 0.9054 | C4—H13 | 0.9737 |
N2—H3 | 0.9132 | C5—H14 | 0.9822 |
N3—H4 | 0.916 | C5—H15 | 0.9722 |
N4—H5 | 0.919 | C6—H16 | 0.9756 |
C1—C2 | 1.5302 | C6—H17 | 0.9807 |
C2—C3 | 1.4958 | C7—H18 | 0.9743 |
C4—C5 | 1.5112 | C7—H19 | 0.9745 |
C6—C7 | 1.5377 | C8—H20 | 0.9749 |
C7—C8 | 1.4833 | C8—H21 | 0.9717 |
C9—C10 | 1.5164 | C9—H22 | 0.9735 |
C10—C11 | 1.4208 | C9—H23 | 0.977 |
C10—C23 | 1.3992 | C12—H24 | 0.9345 |
C11—C12 | 1.4468 | C13—H25 | 0.9304 |
C11—C16 | 1.4295 | C14—H26 | 0.9328 |
C12—C13 | 1.3704 | C15—H27 | 0.9344 |
C13—C14 | 1.3926 | C17—H28 | 0.9341 |
C14—C15 | 1.3645 | C19—H29 | 0.9346 |
C15—C16 | 1.4169 | C20—H30 | 0.9299 |
C16—C17 | 1.4043 | C21—H31 | 0.9331 |
C17—C18 | 1.3807 | C22—H32 | 0.9355 |
| | | |
Cu1···C22 | 3.3948 | H2···H9 | 2.5554 |
Cu1···C23 | 3.6677 | H2···Cl3x | 2.9568 |
Cu1···O1i | 3.781 | H3···Cl1ii | 2.4123 |
Cu1···H18 | 3.6645 | H3···H15 | 2.5069 |
Cu1···H32 | 3.01 | H3···H9 | 2.4386 |
Cu1···H9 | 3.5386 | H4···H18 | 2.396 |
Cl1···O1i | 3.2354 | H4···Cl3 | 2.4975 |
Cl1···N2ii | 3.2535 | H4···H13 | 2.5137 |
Cl3···O1iii | 3.3695 | H5···H24 | 2.5038 |
Cl3···N3 | 3.3713 | H5···C11 | 2.8992 |
Cl1···H16 | 3.0359 | H5···C12 | 2.8987 |
Cl1···H20 | 2.8886 | H5···H1 | 2.2922 |
Cl1···H3ii | 2.4123 | H5···O1i | 2.1903 |
Cl3···H32 | 3.135 | H6···H27vii | 2.4825 |
Cl3···H2iv | 2.9568 | H7···C18 | 2.9831 |
Cl3···H4 | 2.4975 | H7···H10 | 2.4431 |
O1···C2 | 3.3492 | H7···C19 | 3.0796 |
O1···Cl3iii | 3.3695 | H7···C23 | 2.9875 |
O1···Cu1v | 3.781 | H8···O1 | 2.6462 |
O1···Cl1v | 3.2354 | H9···Cu1 | 3.5386 |
O1···N1v | 3.223 | H9···H2 | 2.5554 |
O1···N4v | 3.0138 | H9···H3 | 2.4386 |
O1···H2v | 2.7875 | H10···C21 | 3.0267 |
O1···H5v | 2.1903 | H10···H13 | 2.4153 |
O1···H8 | 2.6462 | H10···H7 | 2.4431 |
N1···O1i | 3.223 | H11···H12 | 2.4782 |
N1···C10 | 3.3769 | H11···C13v | 3.0262 |
N1···C23 | 3.4098 | H12···H30xi | 2.5961 |
N2···Cl1ii | 3.2535 | H12···C19xi | 2.9309 |
N3···Cl3 | 3.3713 | H12···C20xi | 3.0555 |
N4···O1i | 3.0138 | H12···H11 | 2.4782 |
N4···C12 | 3.4299 | H12···H29xi | 2.3274 |
C2···O1 | 3.3492 | H13···H4 | 2.5137 |
C9···C11vi | 3.5578 | H13···H10 | 2.4153 |
C9···C15vi | 3.5841 | H14···H17 | 2.4808 |
C9···C16vi | 3.3761 | H14···H14xii | 2.5202 |
C10···N1 | 3.3769 | H15···H3 | 2.5069 |
C10···C11vi | 3.5286 | H15···H16 | 2.4219 |
C10···C10vi | 3.5318 | H16···H15 | 2.4219 |
C11···C10vi | 3.5286 | H16···Cl1 | 3.0359 |
C11···C9vi | 3.5578 | H16···H20 | 2.486 |
C12···C12vi | 3.555 | H17···H14 | 2.4808 |
C12···N4 | 3.4299 | H18···C9 | 2.7042 |
C15···C9vi | 3.5841 | H18···Cu1 | 3.6645 |
C15···C17vii | 3.3899 | H18···H4 | 2.396 |
C16···C9vi | 3.3761 | H18···H23 | 2.3233 |
C17···C15vii | 3.3899 | H19···H21viii | 2.4512 |
C22···Cu1 | 3.3948 | H20···Cl1 | 2.8886 |
C23···C23vi | 3.5996 | H20···H16 | 2.486 |
C23···Cu1 | 3.6677 | H21···C8viii | 2.8904 |
C23···N1 | 3.4098 | H21···H22 | 2.2116 |
C7···H21viii | 3.0898 | H21···C7viii | 3.0898 |
C7···H23 | 2.9019 | H21···H21viii | 2.3162 |
C8···H21viii | 2.8904 | H21···H19viii | 2.4512 |
C9···H24 | 2.6389 | H22···C12vi | 3.0736 |
C9···H32 | 2.6188 | H22···C11vi | 3.0273 |
C9···H18 | 2.7042 | H22···C12 | 2.6848 |
C10···H1 | 2.687 | H22···H21 | 2.2116 |
C11···H5 | 2.8992 | H22···H24 | 2.1752 |
C11···H1 | 3.0239 | H22···C15vi | 3.0267 |
C11···H22vi | 3.0273 | H22···C16vi | 2.9766 |
C12···H5 | 2.8987 | H22···C14vi | 3.0777 |
C12···H22 | 2.6848 | H23···C16vi | 3.0348 |
C12···H22vi | 3.0736 | H23···H32 | 1.9924 |
C13···H11i | 3.0262 | H23···C7 | 2.9019 |
C14···H22vi | 3.0777 | H23···C22 | 2.5454 |
C15···H28vii | 3.043 | H23···H18 | 2.3233 |
C15···H22vi | 3.0267 | H24···C9 | 2.6389 |
C16···H22vi | 2.9766 | H24···H5 | 2.5038 |
C16···H23vi | 3.0348 | H24···H22 | 2.1752 |
C17···H27vii | 3.0204 | H27···H28 | 2.4464 |
C18···H7 | 2.9831 | H27···C17vii | 3.0204 |
C19···H12ix | 2.9309 | H27···H6vii | 2.4825 |
C19···H7 | 3.0796 | H28···H29 | 2.4133 |
C20···H12ix | 3.0555 | H28···H27 | 2.4464 |
C21···H10 | 3.0267 | H28···C15vii | 3.043 |
C22···H23 | 2.5454 | H29···H12ix | 2.3274 |
C23···H1 | 2.9053 | H29···H28 | 2.4133 |
C23···H7 | 2.9875 | H30···H12ix | 2.5961 |
H1···C10 | 2.687 | H32···H23 | 1.9924 |
H1···C23 | 2.9053 | H32···Cu1 | 3.01 |
H1···H5 | 2.2922 | H32···Cl3 | 3.135 |
H1···C11 | 3.0239 | H32···C9 | 2.6188 |
H2···O1i | 2.7875 | | |
| | | |
Cl1—Cu1—N1 | 89.25 | C10—C23—C18 | 118.8 |
Cl1—Cu1—N2 | 94.83 | C10—C23—C22 | 123.43 |
Cl1—Cu1—N3 | 97.72 | N1—C1—H6 | 109.79 |
Cl1—Cu1—N4 | 94.02 | N1—C1—H7 | 108.67 |
N1—Cu1—N2 | 91.72 | C2—C1—H6 | 108.9 |
N1—Cu1—N3 | 172.47 | C2—C1—H7 | 109.33 |
N1—Cu1—N4 | 92.02 | H6—C1—H7 | 108.64 |
N2—Cu1—N3 | 84.87 | C1—C2—H8 | 108.86 |
N2—Cu1—N4 | 170.43 | C1—C2—H9 | 108.83 |
N3—Cu1—N4 | 90.35 | C3—C2—H8 | 109.48 |
Cu1—N1—C1 | 122.41 | C3—C2—H9 | 109.27 |
Cu1—N2—C3 | 122.16 | H8—C2—H9 | 107.03 |
Cu1—N2—C4 | 106.51 | N2—C3—H10 | 108.31 |
C3—N2—C4 | 111.36 | N2—C3—H11 | 109.15 |
Cu1—N3—C5 | 107.56 | C2—C3—H10 | 109.55 |
Cu1—N3—C6 | 117.53 | C2—C3—H11 | 108.46 |
C5—N3—C6 | 111.27 | H10—C3—H11 | 107.92 |
Cu1—N4—C8 | 114.26 | N2—C4—H12 | 109.57 |
Cu1—N4—C9 | 115.4 | N2—C4—H13 | 110.58 |
C8—N4—C9 | 109.38 | C5—C4—H12 | 110.28 |
Cu1—N1—H2 | 107.57 | C5—C4—H13 | 109.41 |
C1—N1—H1 | 106.89 | H12—C4—H13 | 108.54 |
Cu1—N1—H1 | 106.29 | N3—C5—H14 | 109.66 |
H1—N1—H2 | 106.76 | N3—C5—H15 | 110.14 |
C1—N1—H2 | 106.05 | C4—C5—H14 | 110.59 |
C3—N2—H3 | 104.52 | C4—C5—H15 | 109.43 |
Cu1—N2—H3 | 105.32 | H14—C5—H15 | 108.9 |
C4—N2—H3 | 105.69 | N3—C6—H16 | 108.86 |
Cu1—N3—H4 | 107.29 | N3—C6—H17 | 109.91 |
C5—N3—H4 | 106.64 | C7—C6—H16 | 109.6 |
C6—N3—H4 | 105.96 | C7—C6—H17 | 108.97 |
C9—N4—H5 | 106.09 | H16—C6—H17 | 108.79 |
C8—N4—H5 | 106.04 | C6—C7—H18 | 108.72 |
Cu1—N4—H5 | 104.81 | C6—C7—H19 | 108.75 |
N1—C1—C2 | 111.47 | C8—C7—H18 | 109.13 |
C1—C2—C3 | 113.18 | C8—C7—H19 | 109.05 |
N2—C3—C2 | 113.32 | H18—C7—H19 | 106.79 |
N2—C4—C5 | 108.46 | N4—C8—H20 | 107.89 |
N3—C5—C4 | 108.13 | N4—C8—H21 | 108.83 |
N3—C6—C7 | 110.69 | C7—C8—H20 | 109.28 |
C6—C7—C8 | 114.16 | C7—C8—H21 | 108.05 |
N4—C8—C7 | 114.79 | H20—C8—H21 | 107.79 |
N4—C9—C10 | 111.95 | N4—C9—H22 | 109.3 |
C9—C10—C23 | 119.81 | N4—C9—H23 | 109.53 |
C11—C10—C23 | 120.05 | C10—C9—H22 | 109.38 |
C9—C10—C11 | 120.12 | C10—C9—H23 | 109.55 |
C12—C11—C16 | 116.81 | H22—C9—H23 | 107 |
C10—C11—C12 | 122.82 | C11—C12—H24 | 119.67 |
C10—C11—C16 | 120.25 | C13—C12—H24 | 120.04 |
C11—C12—C13 | 120.29 | C12—C13—H25 | 119.1 |
C12—C13—C14 | 121.73 | C14—C13—H25 | 119.17 |
C13—C14—C15 | 120.23 | C13—C14—H26 | 120.08 |
C14—C15—C16 | 120.45 | C15—C14—H26 | 119.69 |
C11—C16—C17 | 119.07 | C14—C15—H27 | 119.67 |
C11—C16—C15 | 120.44 | C16—C15—H27 | 119.87 |
C15—C16—C17 | 120.48 | C16—C17—H28 | 119.46 |
C16—C17—C18 | 120.9 | C18—C17—H28 | 119.64 |
C17—C18—C23 | 120.74 | C18—C19—H29 | 119.46 |
C17—C18—C19 | 120.04 | C20—C19—H29 | 119.59 |
C19—C18—C23 | 119.22 | C19—C20—H30 | 119.64 |
C18—C19—C20 | 120.95 | C21—C20—H30 | 119.93 |
C19—C20—C21 | 120.43 | C20—C21—H31 | 119.69 |
C20—C21—C22 | 121.08 | C22—C21—H31 | 119.23 |
C21—C22—C23 | 120.52 | C21—C22—H32 | 119.57 |
C18—C23—C22 | 117.76 | C23—C22—H32 | 119.91 |
| | | |
Cl1—Cu1—N1—C1 | −123.16 | C6—C7—C8—N4 | −68.30 |
N2—Cu1—N1—C1 | −28.35 | N4—C9—C10—C23 | −97.65 |
N4—Cu1—N1—C1 | 142.84 | N4—C9—C10—C11 | 81.26 |
Cl1—Cu1—N2—C3 | 118.37 | C23—C10—C11—C12 | 179.76 |
Cl1—Cu1—N2—C4 | −112.21 | C9—C10—C11—C12 | 0.86 |
N1—Cu1—N2—C3 | 28.98 | C9—C10—C11—C16 | 176.71 |
N1—Cu1—N2—C4 | 158.4 | C9—C10—C23—C22 | 1.58 |
N3—Cu1—N2—C3 | −144.29 | C11—C10—C23—C18 | 1.3 |
N3—Cu1—N2—C4 | −14.87 | C11—C10—C23—C22 | −177.33 |
Cl1—Cu1—N3—C5 | 79.79 | C23—C10—C11—C16 | −4.39 |
Cl1—Cu1—N3—C6 | −46.66 | C9—C10—C23—C18 | −179.79 |
N2—Cu1—N3—C5 | −14.41 | C10—C11—C12—C13 | 177.39 |
N2—Cu1—N3—C6 | −140.86 | C10—C11—C16—C17 | 3.77 |
N4—Cu1—N3—C5 | 173.89 | C16—C11—C12—C13 | 1.4 |
N4—Cu1—N3—C6 | 47.45 | C10—C11—C16—C15 | −177.37 |
Cl1—Cu1—N4—C8 | 53.08 | C12—C11—C16—C17 | 179.86 |
Cl1—Cu1—N4—C9 | −178.84 | C12—C11—C16—C15 | −1.28 |
N1—Cu1—N4—C8 | 142.47 | C11—C12—C13—C14 | −1.92 |
N1—Cu1—N4—C9 | −89.45 | C12—C13—C14—C15 | 2.28 |
N3—Cu1—N4—C8 | −44.68 | C13—C14—C15—C16 | −2.11 |
N3—Cu1—N4—C9 | 83.4 | C14—C15—C16—C17 | −179.48 |
Cu1—N1—C1—C2 | 49.57 | C14—C15—C16—C11 | 1.67 |
C3—N2—C4—C5 | 176.4 | C15—C16—C17—C18 | −178.89 |
Cu1—N2—C4—C5 | 41 | C11—C16—C17—C18 | −0.03 |
Cu1—N2—C3—C2 | −52.20 | C16—C17—C18—C23 | −3.07 |
C4—N2—C3—C2 | −179.52 | C16—C17—C18—C19 | 176.24 |
Cu1—N3—C6—C7 | −61.09 | C17—C18—C19—C20 | −179.58 |
C6—N3—C5—C4 | 170.69 | C17—C18—C23—C22 | −178.86 |
Cu1—N3—C5—C4 | 40.64 | C23—C18—C19—C20 | −0.25 |
C5—N3—C6—C7 | 174.3 | C17—C18—C23—C10 | 2.44 |
Cu1—N4—C8—C7 | 61.3 | C19—C18—C23—C22 | 1.82 |
C9—N4—C8—C7 | −69.79 | C19—C18—C23—C10 | −176.88 |
Cu1—N4—C9—C10 | 71.02 | C18—C19—C20—C21 | −1.77 |
C8—N4—C9—C10 | −158.51 | C19—C20—C21—C22 | 2.22 |
N1—C1—C2—C3 | −67.61 | C20—C21—C22—C23 | −0.57 |
C1—C2—C3—N2 | 69.81 | C21—C22—C23—C18 | −1.41 |
N2—C4—C5—N3 | −55.46 | C21—C22—C23—C10 | 177.23 |
N3—C6—C7—C8 | 66.16 | | |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1, −y, −z+1; (iii) −x+1/2, −y+1/2, −z+1/2; (iv) x−1/2, −y, z; (v) −x+1, y+1/2, −z+1/2; (vi) −x+1/2, y, −z; (vii) −x+1, −y, −z; (viii) −x+1/2, −y−1/2, −z+1/2; (ix) x, −y+1/2, z−1/2; (x) x+1/2, −y, z; (xi) x, −y+1/2, z+1/2; (xii) −x+1/2, y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H3···Cl1ii | 0.91 | 2.410 | 3.2535 | 153 |
N3—H4···Cl3 | 0.92 | 2.5 | 3.3713 | 160 |
N4—H5···O1i | 0.92 | 2.19 | 3.0138 | 149 |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) −x+1, −y, −z+1. |
(6) Calcium bis(phenxypenicillin) dihydrate
top
Crystal data top
C32H38CaN4O12S2 | Z = 4 |
Mr = 774.88 | F(000) = 1472 |
Orthorhombic, C2221 | Dx = 1.353 Mg m−3 |
Hall symbol: C 2c 2 | Mo K\a radiation, λ = 0.71070 Å |
a = 19.036 (10) Å | µ = 0.35 mm−1 |
b = 6.508 (2) Å | T = 0 K |
c = 29.178 (18) Å | × × mm |
V = 3615 (3) Å3 | |
Refinement top
0 restraints | |
See text | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
Crystal data top
C32H38CaN4O12S2 | V = 3615 (3) Å3 |
Mr = 774.88 | Z = 4 |
Orthorhombic, C2221 | Mo K\a radiation |
a = 19.036 (10) Å | µ = 0.35 mm−1 |
b = 6.508 (2) Å | T = 0 K |
c = 29.178 (18) Å | × × mm |
Refinement top
0 restraints | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
See text | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca1 | 0.572 | 0.5 | 0 | 0.02* | |
S1 | 0.40325 | 0.65975 | 0.12550 | 0.02* | |
O1 | 0.58275 | 0.18975 | −0.04250 | 0.02* | |
O3 | 0.23325 | 0.37175 | 0.053 | 0.02* | |
O4 | 0.494 | 0.361 | 0.05 | 0.02* | |
O5 | 0.476 | 0.0435 | 0.0735 | 0.02* | |
O6 | 0.166 | 0.889 | 0.0465 | 0.02* | |
O7 | 0.1845 | 0.901 | 0.1675 | 0.02* | |
N1 | 0.35425 | 0.43975 | 0.0575 | 0.02* | |
N2 | 0.258 | 0.817 | 0.091 | 0.02* | |
C1 | 0.38625 | 0.38175 | 0.1375 | 0.02* | |
C2 | 0.38575 | 0.28425 | 0.086 | 0.02* | |
C3 | 0.37425 | 0.65325 | 0.0655 | 0.02* | |
C4 | 0.297 | 0.714 | 0.055 | 0.02* | |
C5 | 0.28375 | 0.47725 | 0.054 | 0.02* | |
C6 | 0.4465 | 0.301 | 0.1675 | 0.02* | |
C7 | 0.315 | 0.356 | 0.16 | 0.02* | |
C8 | 0.45825 | 0.21975 | 0.0685 | 0.02* | |
C9 | 0.19425 | 0.89275 | 0.086 | 0.02* | |
C10 | 0.1605 | 0.9795 | 0.1285 | 0.02* | |
C11 | 0.15725 | 0.71975 | 0.1815 | 0.02* | |
C12 | 0.177 | 0.653 | 0.2225 | 0.02* | |
C13 | 0.152 | 0.471 | 0.24 | 0.02* | |
C14 | 0.107 | 0.353 | 0.2145 | 0.02* | |
C15 | 0.08725 | 0.41675 | 0.1755 | 0.02* | |
C16 | 0.11325 | 0.59525 | 0.154 | 0.02* | |
Geometric parameters (Å, º) top
Ca1—O1 | 2.3783 | N2—C9 | 1.318 |
Ca1—O4 | 2.2697 | C1—C2 | 1.6312 |
S1—C1 | 1.871 | C1—C6 | 1.5355 |
S1—C3 | 1.8361 | C1—C7 | 1.5161 |
O3—C5 | 1.1817 | C2—C8 | 1.5302 |
O4—C8 | 1.2647 | C3—C4 | 1.5533 |
O5—C8 | 1.2046 | C4—C5 | 1.5616 |
O6—C9 | 1.2721 | C9—C10 | 1.5064 |
O7—C10 | 1.3284 | C11—C12 | 1.3271 |
O7—C11 | 1.3518 | C11—C16 | 1.4149 |
N1—C2 | 1.4406 | C12—C13 | 1.3748 |
N1—C3 | 1.4595 | C13—C14 | 1.3701 |
N1—C5 | 1.3679 | C14—C15 | 1.2682 |
N2—C4 | 1.4505 | C15—C16 | 1.41 |
| | | |
S1···O4 | 3.4084 | N2···S1 | 3.1154 |
S1···O5i | 3.2338 | N2···O3 | 3.1381 |
S1···N2 | 3.1154 | N2···O7 | 2.6905 |
O1···O5ii | 2.6929 | N2···N1 | 3.2156 |
O1···O3iii | 2.9089 | N2···C11 | 3.3244 |
O1···O6iv | 3.1687 | C3···O4 | 3.0031 |
O3···N2 | 3.1381 | C3···O5i | 3.2026 |
O3···C9v | 3.346 | C4···C5vi | 3.4246 |
O3···C5vi | 3.4113 | C5···C7 | 3.2469 |
O3···O1vii | 2.9089 | C5···O3vi | 3.4113 |
O4···S1 | 3.4084 | C5···C4vi | 3.4246 |
O4···N1 | 2.718 | C5···C5vi | 3.1651 |
O4···C3 | 3.0031 | C6···O5 | 3.2629 |
O5···S1v | 3.2338 | C6···C16x | 3.4676 |
O5···C3v | 3.2026 | C7···C5 | 3.2469 |
O5···C6 | 3.2629 | C9···O3i | 3.3461 |
O5···O1ii | 2.6929 | C9···C16 | 3.1722 |
O6···O6viii | 3.0742 | C10···C15i | 3.4529 |
O6···O1ix | 3.1687 | C11···N2 | 3.3244 |
O7···N2 | 2.6905 | C15···C10v | 3.4529 |
N1···O4 | 2.718 | C16···C9 | 3.1722 |
N1···N2 | 3.2156 | C16···C6xi | 3.4676 |
| | | |
O1—Ca1—O4 | 93.04 | C6—C1—C7 | 112.55 |
O1—Ca1—O1vi | 170.13 | N1—C2—C1 | 105.13 |
O1—Ca1—O4vi | 93.41 | N1—C2—C8 | 112.06 |
O1—Ca1—O6x | 88.55 | C1—C2—C8 | 114.13 |
O1—Ca1—O6iv | 83.96 | S1—C3—N1 | 104.65 |
O1vi—Ca1—O4 | 93.41 | S1—C3—C4 | 117.83 |
O4—Ca1—O4vi | 98.28 | N1—C3—C4 | 87.93 |
O4—Ca1—O6x | 90.26 | N2—C4—C3 | 117.35 |
O4—Ca1—O6iv | 171.12 | N2—C4—C5 | 112.76 |
O1vi—Ca1—O4vi | 93.04 | C3—C4—C5 | 84.57 |
O1vi—Ca1—O6x | 83.96 | O3—C5—N1 | 134.13 |
O1vi—Ca1—O6iv | 88.55 | O3—C5—C4 | 134.84 |
O4vi—Ca1—O6x | 171.12 | N1—C5—C4 | 90.93 |
O4vi—Ca1—O6iv | 90.26 | O4—C8—O5 | 126.36 |
O6x—Ca1—O6iv | 81.33 | O4—C8—C2 | 115.36 |
C1—S1—C3 | 95.98 | O5—C8—C2 | 118.28 |
Ca1—O4—C8 | 156.36 | O6—C9—N2 | 118.84 |
Ca1xi—O6—C9 | 146.71 | O6—C9—C10 | 124.94 |
C10—O7—C11 | 117.55 | N2—C9—C10 | 116.22 |
C2—N1—C3 | 117.9 | O7—C10—C9 | 114.48 |
C2—N1—C5 | 125.23 | O7—C11—C12 | 116.7 |
C3—N1—C5 | 95.63 | O7—C11—C16 | 123.74 |
C4—N2—C9 | 124.33 | C12—C11—C16 | 119.44 |
S1—C1—C2 | 101.82 | C11—C12—C13 | 121.25 |
S1—C1—C6 | 107.96 | C12—C13—C14 | 119.84 |
S1—C1—C7 | 110.04 | C13—C14—C15 | 119.29 |
C2—C1—C6 | 113.35 | C14—C15—C16 | 124.38 |
C2—C1—C7 | 110.53 | C11—C16—C15 | 115.3 |
| | | |
O1—Ca1—O4—C8 | 7.74 | C4—N2—C9—O6 | −4.92 |
O1vi—Ca1—O4—C8 | −164.78 | C4—N2—C9—C10 | 175.44 |
O4vi—Ca1—O4—C8 | 101.64 | C7—C1—C2—N1 | 81.33 |
O6x—Ca1—O4—C8 | −80.82 | C6—C1—C2—N1 | −151.24 |
C3—S1—C1—C2 | 20.74 | C7—C1—C2—C8 | −155.49 |
C3—S1—C1—C6 | 140.32 | S1—C1—C2—N1 | −35.55 |
C3—S1—C1—C7 | −96.49 | S1—C1—C2—C8 | 87.63 |
C1—S1—C3—C4 | 94.61 | C6—C1—C2—C8 | −28.06 |
C1—S1—C3—N1 | −0.88 | C1—C2—C8—O4 | −85.28 |
Ca1—O4—C8—O5 | 33.53 | C1—C2—C8—O5 | 94.53 |
Ca1—O4—C8—C2 | −146.67 | N1—C2—C8—O4 | 34.06 |
Ca1xi—O6—C9—N2 | −169.99 | N1—C2—C8—O5 | −146.13 |
Ca1xi—O6—C9—C10 | 9.61 | S1—C3—C4—N2 | 14.15 |
C11—O7—C10—C9 | −82.43 | S1—C3—C4—C5 | −98.71 |
C10—O7—C11—C16 | 9.99 | N1—C3—C4—N2 | 119.63 |
C10—O7—C11—C12 | −173.98 | N1—C3—C4—C5 | 6.78 |
C3—N1—C5—C4 | 7.7 | N2—C4—C5—O3 | 51.97 |
C2—N1—C5—C4 | 137.88 | C3—C4—C5—O3 | 169.4 |
C3—N1—C2—C8 | −83.24 | C3—C4—C5—N1 | −7.23 |
C5—N1—C2—C8 | 156.12 | N2—C4—C5—N1 | −124.66 |
C5—N1—C3—S1 | 110.5 | O6—C9—C10—O7 | 155.12 |
C5—N1—C2—C1 | −79.37 | N2—C9—C10—O7 | −25.26 |
C3—N1—C5—O3 | −168.97 | O7—C11—C12—C13 | 179.64 |
C2—N1—C3—S1 | −24.57 | C16—C11—C12—C13 | −4.15 |
C2—N1—C5—O3 | −38.79 | O7—C11—C16—C15 | −176.96 |
C2—N1—C3—C4 | −142.82 | C12—C11—C16—C15 | 7.11 |
C5—N1—C3—C4 | −7.75 | C11—C12—C13—C14 | 1.42 |
C3—N1—C2—C1 | 41.27 | C12—C13—C14—C15 | −2.17 |
C9—N2—C4—C5 | −90.01 | C13—C14—C15—C16 | 5.92 |
C9—N2—C4—C3 | 174.17 | C14—C15—C16—C11 | −8.33 |
Symmetry codes: (i) x, y+1, z; (ii) x, −y, −z; (iii) x+1/2, −y+1/2, −z; (iv) x+1/2, −y+3/2, −z; (v) x, y−1, z; (vi) x, −y+1, −z; (vii) x−1/2, −y+1/2, −z; (viii) x, −y+2, −z; (ix) x−1/2, −y+3/2, −z; (x) x+1/2, y−1/2, z; (xi) x−1/2, y+1/2, z. |
(7) tris(Methyltriethylammonium) bis(dicarbonyl-(4,4',5,5'-tetracyan-2,2'-bi -imidazole-N,
N')-iridium) dicyan-(4,4',5,5'-tetracyan-2,2'-bi-imidazole-N,
N') -platinum acetonitrile solvate.
top
Crystal data top
2(C12IrN8O2−)·(C12N10Pt−)·3(C7H18N+)·3(C2H3N) | Z = 4 |
Mr = see text | F(000) = 1160 |
Orthorhombic, Cmc21 | Dx = 1.785 Mg m−3 |
Hall symbol: C 2c -2 | Mo K\a radiation, λ = 0.71073 Å |
a = 15.151 (19) Å | µ = 6.13 mm−1 |
b = 22.13 (2) Å | T = 0 K |
c = 6.874 (5) Å | × × mm |
V = 2305 (4) Å3 | |
Refinement top
0 restraints | |
See text | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
Crystal data top
2(C12IrN8O2−)·(C12N10Pt−)·3(C7H18N+)·3(C2H3N) | V = 2305 (4) Å3 |
Mr = see text | Z = 4 |
Orthorhombic, Cmc21 | Mo K\a radiation |
a = 15.151 (19) Å | µ = 6.13 mm−1 |
b = 22.13 (2) Å | T = 0 K |
c = 6.874 (5) Å | × × mm |
Refinement top
0 restraints | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
See text | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pt | 0.5 | −0.00199 | 0.75 | 0.02* | |
O1 | 0.37096 | −0.10019 | 0.75005 | 0.02* | |
N1 | 0.41492 | 0.06858 | 0.74534 | 0.02* | |
N2 | 0.3933 | 0.17459 | 0.75046 | 0.02* | |
N3 | 0.16788 | 0.21028 | 0.75020 | 0.02* | |
N4 | 0.20427 | 0.00112 | 0.75 | 0.02* | |
C1 | 0.45421 | 0.12635 | 0.74982 | 0.02* | |
C2 | 0.31665 | 0.1467 | 0.74765 | 0.02* | |
C3 | 0.32796 | 0.0855 | 0.74394 | 0.02* | |
C4 | 0.23525 | 0.18282 | 0.74445 | 0.02* | |
C5 | 0.25801 | 0.03965 | 0.75111 | 0.02* | |
C6 | 0.41741 | −0.06162 | 0.74993 | 0.02* | |
N9 | 0 | 0.13781 | 0.24991 | 0.02* | |
C13 | 0 | 0.20265 | 0.24073 | 0.02* | |
C15 | 0.15324 | 0.13049 | 0.24966 | 0.02* | |
C17 | 0 | 0.10446 | 0.44837 | 0.02* | |
C18 | 0.07478 | 0.11149 | 0.11764 | 0.02* | |
C19 | 0 | 0.03652 | 0.3763 | 0.02* | |
N10 | 0 | 0.23123 | 0.75207 | 0.02* | |
C20 | 0 | 0.18005 | 0.74776 | 0.02* | |
C21 | 0 | 0.11271 | 0.74867 | 0.02* | |
Geometric parameters (Å, º) top
Pt—N1 | 2.0252 | N9—C13 | 1.4363 (18) |
Pt—C6 | 1.8186 | N9—C17 | 1.5511 (19) |
O1—C6 | 1.1063 | N10—C20 | 1.1330 (14) |
N1—C1 | 1.4106 | C1—C1i | 1.3875 |
N1—C3 | 1.3697 | C2—C3 | 1.3654 |
N2—C1 | 1.4111 | C2—C4 | 1.4698 |
N2—C2 | 1.3153 | C3—C5 | 1.468 |
N3—C4 | 1.1886 | C15—C18 | 1.5535 |
N4—C5 | 1.179 | C17—C19 | 1.583 (2) |
N9—C18 | 1.5651 | C20—C21 | 1.4902 (19) |
| | | |
Pt···Ptii | 3.438 (4) | C13···C20xii | 3.425 (4) |
Pt···Ptiii | 3.438 (4) | C13···C20xiii | 3.425 (4) |
Pt···N1ii | 3.9834 | C13···N10xiii | 3.418 (4) |
Pt···N1iii | 3.9277 | C13···N2xiv | 3.162 |
Pt···C6ii | 3.9197 | C13···N2xv | 3.162 |
Pt···C6iii | 3.9188 | C15···C19 | 3.2362 |
Pt···Ptiv | 3.438 (4) | C15···N4iv | 3.0134 |
Pt···Ptv | 3.438 (4) | C15···O1iv | 3.3661 |
Pt···N1iv | 3.9834 | C17···C20 | 2.652 (3) |
Pt···N1v | 3.9277 | C17···C21 | 2.072 (3) |
Pt···C6iv | 3.9197 | C17···C20viii | 2.652 (3) |
Pt···C6v | 3.9188 | C17···C21viii | 2.072 (3) |
O1···C15v | 3.3661 | C18···C20xii | 3.1702 |
N1···Ptii | 3.9277 | C18···C20xiii | 3.1702 |
N1···Ptiii | 3.9834 | C18···C21xii | 2.778 |
N1···Ptiv | 3.9277 | C18···N4iv | 3.2996 |
N1···Ptv | 3.9834 | C18···C21xiii | 2.778 |
N1···C6iv | 3.4091 | C19···C15 | 3.2362 |
N2···N2i | 3.2332 | C19···C21viii | 3.065 (4) |
N2···C13vi | 3.162 | C19···N4iv | 3.3205 |
N2···C13vii | 3.162 | C19···C21iv | 3.417 (4) |
N3···N10 | 2.5855 | C19···C21 | 3.065 (4) |
N3···C20 | 2.6301 | C19···N4xvi | 3.3205 |
N3···C21 | 3.3365 | C19···C21xvi | 3.417 (4) |
N3···N10viii | 2.5855 | C19···C15viii | 3.2362 |
N3···C20viii | 2.6301 | C20···N3 | 2.6301 |
N3···C21viii | 3.3365 | C20···C4 | 3.5649 |
N4···C19ix | 3.3205 | C20···C13 | 3.521 (4) |
N4···C15v | 3.0134 | C20···C13x | 3.425 (4) |
N4···C18v | 3.2996 | C20···C17 | 2.652 (3) |
N4···C19v | 3.3205 | C20···C18x | 3.1702 |
N10···C13x | 3.418 (4) | C20···N3viii | 2.6301 |
N10···N3viii | 2.5855 | C20···C4viii | 3.5649 |
N10···C13xi | 3.418 (4) | C20···C13 | 3.521 (4) |
N10···N3 | 2.5855 | C20···C13xi | 3.425 (4) |
C4···C20 | 3.5649 | C20···C17 | 2.652 (3) |
C4···C20viii | 3.5649 | C20···C18xi | 3.1702 |
C5···C6 | 3.2947 | C21···N3 | 3.3365 |
C6···Ptii | 3.9188 | C21···C17 | 2.072 (3) |
C6···Ptiii | 3.9197 | C21···C18x | 2.778 |
C6···C5 | 3.2947 | C21···C19 | 3.065 (4) |
C6···N1v | 3.4091 | C21···C19ix | 3.417 (4) |
C6···Ptiv | 3.9188 | C21···N3viii | 3.3365 |
C6···Ptv | 3.9197 | C21···C17 | 2.072 (3) |
C13···C20 | 3.521 (4) | C21···C18xi | 2.778 |
C13···C20viii | 3.521 (4) | C21···C19 | 3.065 (4) |
C13···N10xii | 3.418 (4) | C21···C19v | 3.417 (4) |
| | | |
N1—Pt—C6 | 96.98 | N2—C1—C1i | 130.84 |
N1—Pt—N1i | 79.06 | N1—C1—N2 | 114.19 |
N1—Pt—C6i | 175.95 | N1—C1—C1i | 114.96 |
N1i—Pt—C6 | 175.95 | N2—C2—C4 | 119.07 |
C6—Pt—C6i | 86.96 | N2—C2—C3 | 110.79 |
N1i—Pt—C6i | 96.98 | C3—C2—C4 | 130.12 |
Pt—N1—C1 | 115.46 | N1—C3—C5 | 120.35 |
Pt—N1—C3 | 145.4 | N1—C3—C2 | 113.06 |
C1—N1—C3 | 99.11 | C2—C3—C5 | 126.47 |
C1—N2—C2 | 102.85 | N3—C4—C2 | 176.48 |
C17—N9—C18 | 109.5 | N4—C5—C3 | 176.56 |
C17—N9—C18viii | 109.5 | Pt—C6—O1 | 176.03 |
C18—N9—C18viii | 92.75 | N9—C17—C19 | 100.18 |
C13—N9—C18 | 110.26 | N9—C18—C15 | 96.54 |
C13—N9—C18viii | 110.26 | N10—C20—C21 | 178.26 |
C13—N9—C17 | 120.93 | | |
| | | |
C6—Pt—N1—C1 | 178.31 | C1—N2—C2—C4 | −179.11 |
C6—Pt—N1—C3 | 0.73 | C13—N9—C18—C15 | 72.25 |
N1i—Pt—N1—C1 | −2.57 | C13—N9—C17—C19 | 180 |
N1i—Pt—N1—C3 | 179.86 | C18—N9—C17—C19 | −50.17 |
Pt—N1—C1—N2 | −178.77 | C17—N9—C18—C15 | −63.15 |
Pt—N1—C1—C1i | 2.18 | C18viii—N9—C18—C15 | −174.96 |
C3—N1—C1—N2 | −0.16 | N1—C1—C1i—N1i | 0.02 |
C3—N1—C1—C1i | −179.21 | N2—C1—C1i—N1i | −178.86 |
Pt—N1—C3—C2 | 177.65 | N2—C1—C1i—N2i | 0 |
Pt—N1—C3—C5 | 1.45 | N1—C1—C1i—N2i | 178.86 |
C1—N1—C3—C2 | −0.13 | C4—C2—C3—N1 | 178.87 |
C1—N1—C3—C5 | −176.33 | C4—C2—C3—C5 | −5.21 |
C2—N2—C1—N1 | 0.39 | N2—C2—C3—N1 | 0.4 |
C2—N2—C1—C1i | 179.25 | N2—C2—C3—C5 | 176.32 |
C1—N2—C2—C3 | −0.45 | | |
Symmetry codes: (i) −x+1, y, z; (ii) −x+1, −y, z−1/2; (iii) −x+1, −y, z+1/2; (iv) x, −y, z−1/2; (v) x, −y, z+1/2; (vi) −x+1/2, −y+1/2, z+1/2; (vii) x+1/2, −y+1/2, z+1/2; (viii) −x, y, z; (ix) −x, −y, z+1/2; (x) x, y, z+1; (xi) −x, y, z+1; (xii) −x, y, z−1; (xiii) x, y, z−1; (xiv) −x+1/2, −y+1/2, z−1/2; (xv) x−1/2, −y+1/2, z−1/2; (xvi) −x, −y, z−1/2. |
(8) 4-(2-Chloro-4,5-dimethoxybenzylidene)-2-methyl-5-oxazolone
top
Crystal data top
C13H12ClNO4 | Z = 8 |
Mr = 281.69 | F(000) = 1072 |
Orthorhombic, Cmca | Dx = 1.367 Mg m−3 |
Hall symbol: -C 2bc 2 | Mo K\a radiation, λ = 0.71073 Å |
a = 6.707 (1) Å | µ = 0.30 mm−1 |
b = 17.023 (4) Å | T = 0 K |
c = 22.938 (2) Å | × × mm |
V = 2618.9 (8) Å3 | |
Crystal data top
C13H12ClNO4 | V = 2618.9 (8) Å3 |
Mr = 281.69 | Z = 8 |
Orthorhombic, Cmca | Mo K\a radiation |
a = 6.707 (1) Å | µ = 0.30 mm−1 |
b = 17.023 (4) Å | T = 0 K |
c = 22.938 (2) Å | × × mm |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cl1 | 0 | 0.3023 | 0.3021 | 0.02* | |
O1 | 0 | −0.02870 | 0.3698 | 0.02* | |
O2 | 0 | 0.07805 | 0.4488 | 0.02* | |
O3 | 0 | 0.09395 | 0.0695 | 0.02* | |
O4 | 0 | 0.22365 | 0.0885 | 0.02* | |
N1 | 0 | 0.04165 | 0.16 | 0.02* | |
C1 | 0 | 0.2024 | 0.3186 | 0.02* | |
C2 | 0 | 0.1464 | 0.2742 | 0.02* | |
C3 | 0 | 0.06710 | 0.29210 | 0.02* | |
C4 | 0 | 0.04615 | 0.3495 | 0.02* | |
C5 | 0 | 0.10465 | 0.39340 | 0.02* | |
C6 | 0 | 0.1824 | 0.3774 | 0.02* | |
C7 | 0 | −0.08920 | 0.327 | 0.02* | |
C8 | 0 | 0.13575 | 0.4946 | 0.02* | |
C9 | 0 | 0.169 | 0.2135 | 0.02* | |
C10 | 0 | 0.1241 | 0.1658 | 0.02* | |
C11 | 0 | 0.1581 | 0.1065 | 0.02* | |
C12 | 0 | 0.02845 | 0.1055 | 0.02* | |
C13 | 0 | −0.04880 | 0.07460 | 0.02* | |
Geometric parameters (Å, º) top
Cl1—C1 | 1.7422 (4) | C1—C2 | 1.3950 (3) |
O1—C4 | 1.3566 (3) | C1—C6 | 1.3911 (3) |
O1—C7 | 1.4229 (3) | C2—C3 | 1.4110 (3) |
O2—C5 | 1.3490 (3) | C2—C9 | 1.4445 (3) |
O2—C8 | 1.4382 (3) | C3—C4 | 1.3641 (3) |
O3—C11 | 1.3830 (3) | C4—C5 | 1.4162 (3) |
O3—C12 | 1.3875 (3) | C5—C6 | 1.3735 (3) |
O4—C11 | 1.1898 (3) | C9—C10 | 1.3347 (3) |
N1—C10 | 1.4098 (3) | C10—C11 | 1.4782 (3) |
N1—C12 | 1.2702 (3) | C12—C13 | 1.4939 (4) |
| | | |
Cl1···C7i | 3.4901 (8) | C5···C11ix | 3.4747 (8) |
Cl1···C7ii | 3.4901 (8) | C5···C11x | 3.4747 (8) |
O1···O2 | 2.5663 (6) | C5···C12ix | 3.5957 (8) |
O2···O1 | 2.5663 (6) | C5···C12x | 3.5957 (8) |
O3···C13iii | 3.3935 (8) | C6···C11vii | 3.3990 (8) |
O3···C13iv | 3.3935 (8) | C6···C11viii | 3.3990 (8) |
O4···C8v | 3.2199 (8) | C6···C11ix | 3.3990 (8) |
O4···C8vi | 3.2199 (8) | C6···C11x | 3.3990 (8) |
N1···C3 | 3.0609 (7) | C7···Cl1xi | 3.4901 (8) |
N1···C4vii | 3.3614 (8) | C7···Cl1xii | 3.4901 (8) |
N1···C4viii | 3.3614 (8) | C8···O4xiii | 3.2199 (8) |
N1···C4ix | 3.3614 (8) | C8···O4xiv | 3.2199 (8) |
N1···C4x | 3.3614 (8) | C9···C1vii | 3.4801 (8) |
C1···C9vii | 3.4801 (8) | C9···C1viii | 3.4801 (8) |
C1···C9viii | 3.4801 (8) | C9···C2vii | 3.3873 (8) |
C1···C9ix | 3.4801 (8) | C9···C2viii | 3.3873 (8) |
C1···C9x | 3.4801 (8) | C9···C1ix | 3.4801 (8) |
C2···C2vii | 3.5325 (8) | C9···C1x | 3.4801 (8) |
C2···C2viii | 3.5325 (8) | C9···C2ix | 3.3873 (8) |
C2···C9vii | 3.3873 (8) | C9···C2x | 3.3873 (8) |
C2···C9viii | 3.3873 (8) | C11···C5vii | 3.4747 (8) |
C2···C2ix | 3.5325 (8) | C11···C5viii | 3.4747 (8) |
C2···C2x | 3.5325 (8) | C11···C6vii | 3.3990 (8) |
C2···C9ix | 3.3873 (8) | C11···C6viii | 3.3990 (8) |
C2···C9x | 3.3873 (8) | C11···C5ix | 3.4747 (8) |
C3···N1 | 3.0609 (7) | C11···C5x | 3.4747 (8) |
C4···N1vii | 3.3614 (8) | C11···C6ix | 3.3990 (8) |
C4···N1viii | 3.3614 (8) | C11···C6x | 3.3990 (8) |
C4···C12vii | 3.5217 (8) | C12···C4vii | 3.5217 (8) |
C4···C12viii | 3.5217 (8) | C12···C4viii | 3.5217 (8) |
C4···N1ix | 3.3614 (8) | C12···C5vii | 3.5957 (8) |
C4···N1x | 3.3614 (8) | C12···C5viii | 3.5957 (8) |
C4···C12ix | 3.5217 (8) | C12···C4ix | 3.5217 (8) |
C4···C12x | 3.5217 (8) | C12···C4x | 3.5217 (8) |
C5···C11vii | 3.4747 (8) | C12···C5ix | 3.5957 (8) |
C5···C11viii | 3.4747 (8) | C12···C5x | 3.5957 (8) |
C5···C12vii | 3.5957 (8) | C13···O3iii | 3.3935 (8) |
C5···C12viii | 3.5957 (8) | C13···O3iv | 3.3935 (8) |
| | | |
C4—O1—C7 | 116.3 | O2—C5—C4 | 115.71 |
C5—O2—C8 | 117.31 | O2—C5—C6 | 125.11 |
C11—O3—C12 | 105.62 | C4—C5—C6 | 119.18 |
C10—N1—C12 | 105.6 | C1—C6—C5 | 119.67 |
Cl1—C1—C2 | 120.56 | C2—C9—C10 | 129.62 |
Cl1—C1—C6 | 116.71 | N1—C10—C9 | 130.35 |
C2—C1—C6 | 122.73 | N1—C10—C11 | 107.64 |
C1—C2—C3 | 116.19 | C9—C10—C11 | 122.01 |
C1—C2—C9 | 121.45 | O3—C11—O4 | 121.84 |
C3—C2—C9 | 122.36 | O3—C11—C10 | 104.8 |
C2—C3—C4 | 122.07 | O4—C11—C10 | 133.36 |
O1—C4—C3 | 125.23 | O3—C12—N1 | 116.33 |
O1—C4—C5 | 114.61 | O3—C12—C13 | 115.15 |
C3—C4—C5 | 120.16 | N1—C12—C13 | 128.51 |
| | | |
C7—O1—C4—C5 | 180 | C1—C2—C9—C10 | −180.00 |
C7—O1—C4—C3 | 0 | C3—C2—C9—C10 | 0 |
C8—O2—C5—C6 | 0 | C9—C2—C3—C4 | 180 |
C8—O2—C5—C4 | −180.00 | C1—C2—C3—C4 | 0 |
C11—O3—C12—N1 | 0 | C2—C3—C4—O1 | 180 |
C11—O3—C12—C13 | 180 | C2—C3—C4—C5 | 0 |
C12—O3—C11—C10 | 0 | O1—C4—C5—O2 | 0 |
C12—O3—C11—O4 | 180 | C3—C4—C5—O2 | 180 |
C12—N1—C10—C11 | 0 | O1—C4—C5—C6 | −180.00 |
C12—N1—C10—C9 | −180.00 | C3—C4—C5—C6 | 0 |
C10—N1—C12—O3 | 0 | C4—C5—C6—C1 | 0 |
C10—N1—C12—C13 | −180.00 | O2—C5—C6—C1 | 180 |
Cl1—C1—C6—C5 | 180 | C2—C9—C10—C11 | 180 |
Cl1—C1—C2—C3 | −180.00 | C2—C9—C10—N1 | 0 |
Cl1—C1—C2—C9 | 0 | C9—C10—C11—O4 | 0 |
C2—C1—C6—C5 | 0 | N1—C10—C11—O3 | 0 |
C6—C1—C2—C9 | −180.00 | N1—C10—C11—O4 | −180.00 |
C6—C1—C2—C3 | 0 | C9—C10—C11—O3 | 180 |
Symmetry codes: (i) −x, y+1/2, −z+1/2; (ii) x, y+1/2, −z+1/2; (iii) x, −y, −z; (iv) −x, −y, −z; (v) −x, −y+1/2, z−1/2; (vi) x, −y+1/2, z−1/2; (vii) −x−1/2, y, −z+1/2; (viii) −x+1/2, y, −z+1/2; (ix) x−1/2, y, −z+1/2; (x) x+1/2, y, −z+1/2; (xi) −x, y−1/2, −z+1/2; (xii) x, y−1/2, −z+1/2; (xiii) −x, −y+1/2, z+1/2; (xiv) x, −y+1/2, z+1/2. |
(9) Insine 5'-monphosphate nnahydrate
top
Crystal data top
C10H12N4O8P·2.5(H2O)·8(H2O) | Z = 8 |
Mr = 536.38 | F(000) = 2272 |
Orthorhombic, C2221 | Dx = 1.621 Mg m−3 |
Hall symbol: C 2c 2 | Mo K\a radiation, λ = 0.71073 Å |
a = 23.1914 (10) Å | µ = 0.22 mm−1 |
b = 8.650 (1) Å | T = 0 K |
c = 21.900 (1) Å | × × mm |
V = 4393.3 (6) Å3 | |
Refinement top
0 restraints | |
See text | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
Crystal data top
C10H12N4O8P·2.5(H2O)·8(H2O) | V = 4393.3 (6) Å3 |
Mr = 536.38 | Z = 8 |
Orthorhombic, C2221 | Mo K\a radiation |
a = 23.1914 (10) Å | µ = 0.22 mm−1 |
b = 8.650 (1) Å | T = 0 K |
c = 21.900 (1) Å | × × mm |
Refinement top
0 restraints | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
See text | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
P1 | 0.12285 | 0.11165 | 0.2228 | 0.02* | |
O1 | 0.09027 | 0.00897 | 0.1788 | 0.02* | |
O2 | 0.19038 | 0.10198 | 0.2032 | 0.02* | |
O3 | 0.10808 | 0.28018 | 0.21455 | 0.02* | |
O4 | 0.1186 | 0.05475 | 0.28705 | 0.02* | |
O5 | 0.27233 | −0.02242 | 0.1171 | 0.02* | |
O6 | 0.36817 | 0.27928 | 0.1555 | 0.02* | |
O7 | 0.3752 | −0.00210 | 0.2031 | 0.02* | |
O8 | 0.24465 | 0.43745 | −0.12720 | 0.02* | |
N1 | 0.2794 | 0.1908 | 0.0529 | 0.02* | |
N2 | 0.21102 | 0.30508 | −0.00200 | 0.02* | |
N3 | 0.36167 | 0.22767 | −0.01370 | 0.02* | |
N4 | 0.33413 | 0.35833 | −0.10370 | 0.02* | |
C1 | 0.21635 | −0.04615 | 0.21065 | 0.02* | |
C2 | 0.27540 | −0.05215 | 0.1825 | 0.02* | |
C3 | 0.30827 | 0.10012 | 0.10215 | 0.02* | |
C4 | 0.31697 | 0.19173 | 0.16070 | 0.02* | |
C5 | 0.31955 | 0.0621 | 0.2074 | 0.02* | |
C6 | 0.22312 | 0.22523 | 0.04925 | 0.02* | |
C7 | 0.26235 | 0.31375 | −0.03120 | 0.02* | |
C8 | 0.30602 | 0.24072 | 0.00120 | 0.02* | |
C9 | 0.37225 | 0.28225 | −0.06795 | 0.02* | |
C10 | 0.27643 | 0.37638 | −0.09065 | 0.02* | |
O25 | 0.03565 | 0.01155 | 0.3171 | 0.02* | 0.5 |
O27 | 0.02365 | −0.05735 | 0.33945 | 0.02* | |
O28 | 0.02108 | 0.08377 | 0.3542 | 0.02* | |
O17 | 0.041 | 0.64355 | 0.3152 | 0.02* | |
O19 | 0.0573 | 0.7091 | 0.20015 | 0.02* | |
O21 | 0.12765 | 0.5 | 0 | 0.02* | 0.5 |
O22 | 0.12888 | 0.50378 | 0.12845 | 0.02* | |
O23 | 0 | 0.4153 | 0.25 | 0.02* | 0.5 |
O26 | 0.115 | 0.91725 | 0.0637 | 0.02* | |
O31 | 0.46338 | 0.12762 | 0.066 | 0.02* | |
O32 | 0.47328 | 0.35322 | 0.054 | 0.02* | |
O35 | 0.0413 | 0.344 | 0.421 | 0.02* | 0.5 |
O36 | 0.05065 | 0.62575 | 0.0712 | 0.02* | 0.5 |
Geometric parameters (Å, º) top
P1—O1 | 1.5127 | N1—C3 | 1.4923 |
P1—O2 | 1.626 | N2—C6 | 1.3474 |
P1—O3 | 1.5083 | N2—C7 | 1.3534 |
P1—O4 | 1.4939 | N3—C9 | 1.3018 |
O2—C1 | 1.4252 | N3—C8 | 1.336 |
O5—C2 | 1.4569 | N4—C9 | 1.3519 |
O5—C3 | 1.3876 | N4—C10 | 1.3772 |
O6—C4 | 1.4129 | C1—C2 | 1.5027 |
O7—C5 | 1.4082 | C2—C5 | 1.5239 |
O8—C10 | 1.2095 | C3—C4 | 1.5208 |
O25—O28 | 1.0792 | C4—C5 | 1.5188 |
N1—C6 | 1.3411 | C7—C8 | 1.3886 |
N1—C8 | 1.36 | C7—C10 | 1.4475 |
| | | |
P1···O25 | 3.0173 | O22···O21 | 2.8134 |
O1···O19i | 2.7443 | O23···O17 | 2.6155 |
O1···O26i | 2.7041 | O23···O19 | 3.0686 |
O1···O25ii | 2.9217 | O23···O3ii | 2.8725 |
O1···O28ii | 2.7585 | O23···O19ii | 3.0686 |
O2···O5 | 2.8854 | O23···O3 | 2.8725 |
O2···C4 | 3.1761 | O23···O7iii | 3.1531 |
O3···O22 | 2.7439 | O25···O32v | 3.1444 |
O3···O23 | 2.8725 | O25···O4 | 2.0672 |
O3···O23ii | 2.8725 | O25···P1 | 3.0173 |
O3···O7iii | 2.6362 | O25···O6v | 3.0614 |
O3···C5iii | 3.4184 | O25···O1ii | 2.9217 |
O4···O25 | 2.0672 | O25···O17i | 3.1859 |
O4···O28 | 2.7094 | O26···N2viii | 3.2378 |
O4···N4iv | 2.7371 | O26···O36 | 2.9346 |
O4···O6v | 2.712 | O28···O1ii | 2.7585 |
O5···O2 | 2.8854 | O28···O35 | 2.7252 |
O5···O7 | 3.0446 | O28···O4 | 2.7094 |
O5···N4vi | 3.2531 | O28···C9iv | 3.2202 |
O5···C7vi | 3.1532 | O28···O32v | 2.8348 |
O5···C8vi | 3.2997 | O31···O32 | 1.9824 |
O5···C9vi | 3.4029 | O31···O6 | 3.2308 |
O5···C10vi | 3.1175 | O31···O35x | 3.1868 |
O6···O7 | 2.6528 | O31···O17v | 2.6073 |
O6···O31 | 3.2308 | O31···N3 | 3.0593 |
O6···N1 | 3.1421 | O32···O28iii | 2.8348 |
O6···O4iii | 2.712 | O32···O25iii | 3.1444 |
O6···O17v | 2.4955 | O32···O31 | 1.9824 |
O6···O25iii | 3.0614 | O32···N3 | 3.1745 |
O7···O5 | 3.0446 | O35···O28 | 2.7252 |
O7···O6 | 2.6528 | O35···O31iii | 2.4722 |
O7···O23vii | 3.1531 | O35···N3iv | 2.7374 |
O7···O3v | 2.6362 | O35···C9iv | 2.2958 |
O7···O17v | 2.3505 | O36···O26 | 2.9346 |
O7···O19v | 3.2058 | O36···O19 | 2.9187 |
O7···O23v | 3.1531 | O36···O21 | 2.6083 |
O8···N2 | 3.072 | O36···O22 | 2.4447 |
O8···O22viii | 2.7327 | O36···O21viii | 2.6083 |
O8···C6viii | 3.4172 | N1···O6 | 3.1421 |
O17···C5iii | 3.3467 | N2···O21 | 2.5657 |
O17···O25ix | 3.1859 | N2···O21viii | 2.5657 |
O17···O19ii | 2.3731 | N2···O8 | 3.072 |
O17···O23ii | 2.6155 | N2···O26viii | 3.2378 |
O17···O6iii | 2.4955 | N3···O32 | 3.1745 |
O17···O7iii | 2.3505 | N3···O35x | 2.7374 |
O17···O19 | 2.6101 | N3···O31 | 3.0593 |
O17···O23 | 2.6155 | N4···C2vi | 3.442 |
O17···C4iii | 3.3618 | N4···O4x | 2.7371 |
O17···O31iii | 2.6073 | N4···O5vi | 3.2531 |
O19···O22 | 2.8941 | C2···C10vi | 3.4514 |
O19···O17 | 2.6101 | C2···N4vi | 3.442 |
O19···O23ii | 3.0686 | C4···O17v | 3.3618 |
O19···O23 | 3.0686 | C4···O2 | 3.1761 |
O19···O36 | 2.9187 | C5···O3v | 3.4184 |
O19···O7iii | 3.2058 | C5···O17v | 3.3467 |
O21···O36 | 2.6083 | C6···O8viii | 3.4172 |
O21···N2 | 2.5657 | C7···O5vi | 3.1532 |
O21···O22 | 2.8134 | C7···C7viii | 3.4999 |
O21···N2viii | 2.5657 | C8···O5vi | 3.2997 |
O21···O22viii | 2.8134 | C9···O5vi | 3.4029 |
O22···O3 | 2.7439 | C9···O28x | 3.2202 |
O22···O21viii | 2.8134 | C9···O35x | 2.2958 |
O22···O8viii | 2.7327 | C10···O5vi | 3.1175 |
O22···O36 | 2.4447 | C10···C2vi | 3.4514 |
O22···O19 | 2.8941 | | |
| | | |
O1—P1—O2 | 106.42 | O5—C3—C4 | 106.19 |
O1—P1—O3 | 112.19 | N1—C3—C4 | 113.27 |
O1—P1—O4 | 111.94 | O6—C4—C3 | 108.83 |
O2—P1—O3 | 103.7 | O6—C4—C5 | 114.64 |
O2—P1—O4 | 107.17 | C3—C4—C5 | 100.85 |
O3—P1—O4 | 114.6 | O7—C5—C2 | 109.64 |
P1—O2—C1 | 115.03 | O7—C5—C4 | 106.39 |
C2—O5—C3 | 109.72 | C2—C5—C4 | 102.2 |
C3—N1—C6 | 126.62 | N1—C6—N2 | 111.48 |
C3—N1—C8 | 124.4 | N2—C7—C8 | 112.02 |
C6—N1—C8 | 108.76 | N2—C7—C10 | 130.1 |
C6—N2—C7 | 103.82 | C8—C7—C10 | 117.73 |
C8—N3—C9 | 111.98 | N1—C8—N3 | 127.95 |
C9—N4—C10 | 124.78 | N1—C8—C7 | 103.81 |
O2—C1—C2 | 111.67 | N3—C8—C7 | 128.18 |
O5—C2—C1 | 110.65 | N3—C9—N4 | 125.58 |
O5—C2—C5 | 105.67 | O8—C10—N4 | 120.28 |
C1—C2—C5 | 116.3 | O8—C10—C7 | 128.41 |
O5—C3—N1 | 107.61 | N4—C10—C7 | 111.31 |
| | | |
O1—P1—O2—C1 | −65.28 | C9—N4—C10—C7 | 4.48 |
O3—P1—O2—C1 | 176.22 | C9—N4—C10—O8 | −175.11 |
O4—P1—O2—C1 | 54.64 | O2—C1—C2—C5 | 59.59 |
P1—O2—C1—C2 | 170.96 | O2—C1—C2—O5 | −60.96 |
C3—O5—C2—C5 | −2.20 | O5—C2—C5—C4 | 25.23 |
C2—O5—C3—N1 | −143.71 | C1—C2—C5—O7 | 149.48 |
C3—O5—C2—C1 | 124.49 | C1—C2—C5—C4 | −97.95 |
C2—O5—C3—C4 | −22.12 | O5—C2—C5—O7 | −87.34 |
C3—N1—C8—N3 | −4.29 | O5—C3—C4—O6 | 158.08 |
C6—N1—C8—N3 | −179.19 | N1—C3—C4—O6 | −84.03 |
C6—N1—C8—C7 | 3.15 | O5—C3—C4—C5 | 37.16 |
C6—N1—C3—O5 | 40.54 | N1—C3—C4—C5 | 155.05 |
C3—N1—C6—N2 | −178.22 | O6—C4—C5—O7 | −38.56 |
C3—N1—C8—C7 | 178.05 | O6—C4—C5—C2 | −153.52 |
C8—N1—C3—C4 | 109.51 | C3—C4—C5—O7 | 78.15 |
C8—N1—C3—O5 | −133.44 | C3—C4—C5—C2 | −36.81 |
C6—N1—C3—C4 | −76.51 | C10—C7—C8—N3 | 4.42 |
C8—N1—C6—N2 | −3.47 | N2—C7—C10—O8 | 1.15 |
C7—N2—C6—N1 | 2.14 | N2—C7—C10—N4 | −178.40 |
C6—N2—C7—C8 | −0.08 | C8—C7—C10—O8 | 176.32 |
C6—N2—C7—C10 | 175.32 | C8—C7—C10—N4 | −3.22 |
C8—N3—C9—N4 | 6.57 | N2—C7—C8—N1 | −1.91 |
C9—N3—C8—N1 | 177.21 | N2—C7—C8—N3 | −179.56 |
C9—N3—C8—C7 | −5.68 | C10—C7—C8—N1 | −177.92 |
C10—N4—C9—N3 | −6.82 | | |
Symmetry codes: (i) x, y−1, z; (ii) −x, y, −z+1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x+1/2, −y+1/2, z+1/2; (v) −x+1/2, y−1/2, −z+1/2; (vi) x, −y, −z; (vii) x+1/2, y−1/2, z; (viii) x, −y+1, −z; (ix) x, y+1, z; (x) −x+1/2, −y+1/2, z−1/2. |
(10)
catena-((mu!2$-Acetato-
O,
O')-(acetato-
O,
O')-(pyridine)-zinc(ii))
top
Crystal data top
C18H22N2O8Zn2 | γ = 90° |
Mr = 525.16 | V = 2181.2 (11) Å3 |
Monclinic, P21/n | Z = 4 |
Hall symbol: -P 2yn | F(000) = 984 |
a = 8.626 (2) Å | Dx = 1.532 Mg m−3 |
b = 28.871 (8) Å | Mo K\a radiation, λ = 0.71073 Å |
c = 8.868 (3) Å | µ = 2.24 mm−1 |
α = 90° | T = 0 K |
β = 99.02 (2)° | × × mm |
Crystal data top
C18H22N2O8Zn2 | γ = 90° |
Mr = 525.16 | V = 2181.2 (11) Å3 |
Monclinic, P21/n | Z = 4 |
a = 8.626 (2) Å | Mo K\a radiation |
b = 28.871 (8) Å | µ = 2.24 mm−1 |
c = 8.868 (3) Å | T = 0 K |
α = 90° | × × mm |
β = 99.02 (2)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Zn3 | 0.3766 | 0.10455 | 0.4451 | 0.02* | |
Zn4 | 0.36455 | 0.1493 | −0.06510 | 0.02* | |
O1 | 0.40265 | 0.04545 | 0.32695 | 0.02* | |
O2 | 0.1564 | 0.05875 | 0.3237 | 0.02* | |
O3 | 0.3963 | 0.21215 | −0.17870 | 0.02* | |
O4 | 0.16295 | 0.1895 | −0.19330 | 0.02* | |
O5 | 0.27855 | 0.16465 | 0.3807 | 0.02* | |
O6 | 0.3374 | 0.1504 | 0.15385 | 0.02* | |
O7 | 0.3472 | 0.10235 | 0.66220 | 0.02* | |
O8 | 0.2784 | 0.08605 | 0.8828 | 0.02* | |
N1 | 0.6127 | 0.11995 | 0.48105 | 0.02* | |
N2 | 0.60040 | 0.13330 | −0.02655 | 0.02* | |
C1 | 0.26205 | 0.03625 | 0.2767 | 0.02* | |
C2 | 0.2311 | −0.00030 | 0.1591 | 0.02* | |
C3 | 0.25935 | 0.2165 | −0.23535 | 0.02* | |
C4 | 0.2082 | 0.25235 | −0.35235 | 0.02* | |
C5 | 0.27595 | 0.1753 | 0.24315 | 0.02* | |
C6 | 0.19755 | 0.2199 | 0.18915 | 0.02* | |
C7 | 0.2951 | 0.07475 | 0.7503 | 0.02* | |
C8 | 0.2552 | 0.02615 | 0.69985 | 0.02* | |
C9 | 0.67145 | 0.1628 | 0.4682 | 0.02* | |
C10 | 0.8296 | 0.17120 | 0.4867 | 0.02* | |
C11 | 0.93365 | 0.13510 | 0.51655 | 0.02* | |
C12 | 0.87435 | 0.09155 | 0.52915 | 0.02* | |
C13 | 0.716 | 0.0849 | 0.51155 | 0.02* | |
C14 | 0.69880 | 0.15255 | −0.11150 | 0.02* | |
C15 | 0.85755 | 0.14375 | −0.08780 | 0.02* | |
C16 | 0.91815 | 0.1142 | 0.02365 | 0.02* | |
C17 | 0.81495 | 0.09350 | 0.11525 | 0.02* | |
C18 | 0.6615 | 0.1041 | 0.084 | 0.02* | |
Geometric parameters (Å, º) top
Zn3—O1 | 2.0331 | O8—C7 | 1.2494 |
Zn3—O2 | 2.4237 | N1—C9 | 1.3485 |
Zn3—O5 | 1.975 | N1—C13 | 1.3474 |
Zn3—O7 | 1.9819 | N2—C14 | 1.3407 |
Zn3—N1 | 2.06 | N2—C18 | 1.337 |
Zn4—O3 | 2.114 | C1—C2 | 1.4782 |
Zn4—O4 | 2.2458 | C3—C4 | 1.4829 |
Zn4—O6 | 1.9921 | C5—C6 | 1.4977 |
Zn4—N2 | 2.0618 | C7—C8 | 1.4964 |
Zn4—O8i | 1.9982 | C9—C10 | 1.3699 |
O1—C1 | 1.2532 | C10—C11 | 1.3738 |
O2—C1 | 1.2431 | C11—C12 | 1.3686 |
O3—C3 | 1.2156 | C12—C13 | 1.3639 |
O4—C3 | 1.2391 | C14—C15 | 1.3761 |
O5—C5 | 1.2547 | C15—C16 | 1.3476 |
O6—C5 | 1.2476 | C16—C17 | 1.427 |
O7—C7 | 1.248 | C17—C18 | 1.3444 |
| | | |
Zn3···Zn4 | 4.6908 | O4···C15iii | 3.2145 |
Zn3···Zn4ii | 4.5484 | C4···C14v | 3.5732 |
Zn3···C11iii | 4.0667 | C11···Zn3vi | 4.0667 |
Zn4···Zn3i | 4.5484 | C11···O4vii | 3.3769 |
Zn4···Zn3 | 4.6908 | C12···O2vi | 3.3949 |
O2···C12iii | 3.3949 | C14···C4viii | 3.5732 |
O2···C17iii | 3.3751 | C15···O4vi | 3.2145 |
O4···C11iv | 3.3769 | C17···O2vi | 3.3751 |
| | | |
O1—Zn3—O2 | 57.01 | Zn3—N1—C9 | 124.09 |
O1—Zn3—O5 | 131.7 | Zn3—N1—C13 | 118.4 |
O1—Zn3—O7 | 121 | C9—N1—C13 | 117.42 |
O1—Zn3—N1 | 94.27 | Zn4—N2—C14 | 120.61 |
O2—Zn3—O5 | 94.62 | Zn4—N2—C18 | 121.88 |
O2—Zn3—O7 | 101.73 | C14—N2—C18 | 117.51 |
O2—Zn3—N1 | 150.86 | O1—C1—O2 | 119.31 |
O5—Zn3—O7 | 101.23 | O1—C1—C2 | 117.38 |
O5—Zn3—N1 | 102.9 | O2—C1—C2 | 123.28 |
O7—Zn3—N1 | 97.5 | O3—C3—O4 | 117.72 |
O3—Zn4—O4 | 57.52 | O3—C3—C4 | 121.64 |
O3—Zn4—O6 | 119.64 | O4—C3—C4 | 120.63 |
O3—Zn4—N2 | 94.19 | O5—C5—O6 | 122.09 |
O3—Zn4—O8i | 138.2 | O5—C5—C6 | 117.38 |
O4—Zn4—O6 | 106.57 | O6—C5—C6 | 120.53 |
O4—Zn4—N2 | 149.92 | O7—C7—O8 | 121.87 |
O4—Zn4—O8i | 97.17 | O7—C7—C8 | 120.01 |
O6—Zn4—N2 | 96.07 | O8—C7—C8 | 118.1 |
O6—Zn4—O8i | 98.26 | N1—C9—C10 | 122.19 |
O8i—Zn4—N2 | 98.92 | C9—C10—C11 | 119.8 |
Zn3—O1—C1 | 100.49 | C10—C11—C12 | 118.13 |
Zn3—O2—C1 | 82.49 | C11—C12—C13 | 120.03 |
Zn4—O3—C3 | 95.48 | N1—C13—C12 | 122.42 |
Zn4—O4—C3 | 88.54 | N2—C14—C15 | 122.7 |
Zn3—O5—C5 | 115.97 | C14—C15—C16 | 119.42 |
Zn4—O6—C5 | 138.98 | C15—C16—C17 | 118.54 |
Zn3—O7—C7 | 137.91 | C16—C17—C18 | 117.98 |
Zn4ii—O8—C7 | 111.26 | N2—C18—C17 | 123.84 |
| | | |
O2—Zn3—O1—C1 | 4.85 | O3—Zn4—N2—C14 | −20.96 |
O5—Zn3—O1—C1 | −58.42 | O4—Zn4—N2—C14 | −2.32 |
O7—Zn3—O1—C1 | 88.69 | O6—Zn4—N2—C14 | −141.39 |
N1—Zn3—O1—C1 | −169.92 | O8i—Zn4—N2—C14 | 119.23 |
O1—Zn3—O2—C1 | −4.85 | O3—Zn4—N2—C18 | 158.21 |
O5—Zn3—O2—C1 | 133.15 | O4—Zn4—N2—C18 | 176.86 |
O7—Zn3—O2—C1 | −124.35 | O6—Zn4—N2—C18 | 37.78 |
N1—Zn3—O2—C1 | 5.91 | O8i—Zn4—N2—C18 | −61.60 |
O7—Zn3—N1—C13 | 83.43 | Zn3—O1—C1—O2 | −9.13 |
O1—Zn3—O7—C7 | −26.17 | Zn3—O1—C1—C2 | 168.83 |
O2—Zn3—O7—C7 | 32.23 | Zn3—O2—C1—O1 | 7.58 |
O5—Zn3—O7—C7 | 129.42 | Zn3—O2—C1—C2 | −170.25 |
N1—Zn3—O7—C7 | −125.76 | Zn4—O3—C3—O4 | 8.71 |
O7—Zn3—N1—C9 | −100.20 | Zn4—O3—C3—C4 | −170.51 |
O1—Zn3—N1—C13 | −38.63 | Zn4—O4—C3—O3 | −8.16 |
O2—Zn3—N1—C13 | −47.67 | Zn4—O4—C3—C4 | 171.07 |
O1—Zn3—O5—C5 | −26.62 | Zn3—O5—C5—O6 | −2.91 |
O2—Zn3—O5—C5 | −75.34 | Zn3—O5—C5—C6 | 177.96 |
O7—Zn3—O5—C5 | −178.29 | Zn4—O6—C5—O5 | 178.57 |
N1—Zn3—O5—C5 | 81.22 | Zn4—O6—C5—C6 | −2.34 |
O5—Zn3—N1—C9 | 3.21 | Zn3—O7—C7—O8 | −172.66 |
O1—Zn3—N1—C9 | 137.75 | Zn3—O7—C7—C8 | 9.19 |
O5—Zn3—N1—C13 | −173.17 | Zn4ii—O8—C7—O7 | −5.68 |
O2—Zn3—N1—C9 | 128.71 | Zn4ii—O8—C7—C8 | 172.5 |
N2—Zn4—O4—C3 | −17.29 | Zn3—N1—C9—C10 | −177.13 |
O6—Zn4—O3—C3 | −96.56 | C13—N1—C9—C10 | −0.72 |
O8i—Zn4—O4—C3 | −139.24 | Zn3—N1—C13—C12 | 176.57 |
O6—Zn4—O4—C3 | 119.89 | C9—N1—C13—C12 | −0.05 |
O3ii—Zn4ii—O8—C7 | 30.17 | C18—N2—C14—C15 | −0.71 |
O4ii—Zn4ii—O8—C7 | 78.01 | Zn4—N2—C14—C15 | 178.49 |
O6ii—Zn4ii—O8—C7 | −174.01 | C14—N2—C18—C17 | 0.72 |
N2ii—Zn4ii—O8—C7 | −76.49 | Zn4—N2—C18—C17 | −178.47 |
N2—Zn4—O3—C3 | 164.02 | N1—C9—C10—C11 | 1.26 |
O8i—Zn4—O3—C3 | 55.64 | C9—C10—C11—C12 | −0.99 |
O3—Zn4—O4—C3 | 4.91 | C10—C11—C12—C13 | 0.26 |
O3—Zn4—O6—C5 | 35.3 | C11—C12—C13—N1 | 0.27 |
O4—Zn4—O6—C5 | −26.32 | N2—C14—C15—C16 | 0.87 |
N2—Zn4—O6—C5 | 133.65 | C14—C15—C16—C17 | −0.95 |
O8i—Zn4—O6—C5 | −126.39 | C15—C16—C17—C18 | 0.94 |
O4—Zn4—O3—C3 | −5.03 | C16—C17—C18—N2 | −0.84 |
Symmetry codes: (i) x, y, z−1; (ii) x, y, z+1; (iii) x−1, y, z; (iv) x−1, y, z−1; (v) x−1/2, −y+1/2, z−1/2; (vi) x+1, y, z; (vii) x+1, y, z+1; (viii) x+1/2, −y+1/2, z+1/2. |
(11) bis(Pyridine)-tetra-aqua-iron(ii) diacetate
top
Crystal data top
C10H18FeN2O4·2(C2H3O2) | γ = 90° |
Mr = 404.20 | V = 934.5 (3) Å3 |
Monclinic, I2/m | Z = 2 |
Hall symbol: -I 2y | F(000) = 376 |
a = 11.780 (2) Å | Dx = 1.350 Mg m−3 |
b = 9.734 (2) Å | Mo K\a radiation, λ = 0.71070 Å |
c = 8.401 (2) Å | µ = 0.85 mm−1 |
α = 90° | T = 0 K |
β = 104.05 (2)° | × × mm |
Crystal data top
C10H18FeN2O4·2(C2H3O2) | γ = 90° |
Mr = 404.20 | V = 934.5 (3) Å3 |
Monclinic, I2/m | Z = 2 |
a = 11.780 (2) Å | Mo K\a radiation |
b = 9.734 (2) Å | µ = 0.85 mm−1 |
c = 8.401 (2) Å | T = 0 K |
α = 90° | × × mm |
β = 104.05 (2)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe1 | 0 | 0 | 1 | 0.02* | |
O1 | −0.12083 | 0.15453 | 0.89028 | 0.02* | |
N1 | 0.0866 | 0 | 0.7939 | 0.02* | |
C1 | 0.1102 | 0.11555 | 0.72515 | 0.02* | |
C2 | 0.15573 | 0.12008 | 0.58847 | 0.02* | |
C3 | 0.1778 | 0 | 0.5195 | 0.02* | |
O3 | 0.35263 | 0.11323 | 0.19853 | 0.02* | |
C6 | 0.401 | 0 | 0.22 | 0.02* | |
C7 | 0.53195 | 0 | 0.27875 | 0.02* | |
Geometric parameters (Å, º) top
Fe1—O1 | 2.1216 | N1—C1 | 1.3244 |
Fe1—N1 | 2.2127 (5) | C1—C2 | 1.381 |
Fe1—N1i | 2.2127 (5) | C2—C3 | 1.3575 |
O3—C6 | 1.2337 | C6—C7 | 1.5012 (4) |
| | | |
O1···O3ii | 2.6805 | C2···C1ii | 3.5707 |
O1···O3iii | 2.7493 | C3···C7v | 3.4278 (8) |
O3···O1ii | 2.6805 | C3···C7vi | 3.4278 (8) |
O3···O1iv | 2.7493 | C7···C3vi | 3.4278 (8) |
C1···C2ii | 3.5707 | C7···C3v | 3.4278 (8) |
| | | |
O1—Fe1—N1 | 92.76 | O1vii—Fe1—N1i | 92.76 |
O1—Fe1—O1i | 89.69 | O1viii—Fe1—N1i | 87.24 |
O1—Fe1—N1i | 87.24 | O1vii—Fe1—O1viii | 89.69 |
O1—Fe1—O1vii | 180 | Fe1—N1—C1 | 121.78 |
O1—Fe1—O1viii | 90.31 | Fe1—N1—C1viii | 121.78 |
O1i—Fe1—N1 | 87.24 | C1—N1—C1viii | 116.27 |
N1—Fe1—N1i | 180 | N1—C1—C2 | 123.69 |
O1vii—Fe1—N1 | 87.24 | C1—C2—C3 | 118.73 |
O1viii—Fe1—N1 | 92.76 | C2—C3—C2viii | 118.87 |
O1i—Fe1—N1i | 92.76 | O3—C6—C7 | 116.7 |
O1i—Fe1—O1vii | 90.31 | O3—C6—O3viii | 126.6 |
O1i—Fe1—O1viii | 180 | O3viii—C6—C7 | 116.7 |
| | | |
O1—Fe1—N1—C1 | 42.37 | Fe1—N1—C1—C2 | −174.78 |
O1—Fe1—N1—C1viii | −132.81 | C1viii—N1—C1—C2 | 0.65 |
O1i—Fe1—N1—C1 | −47.19 | N1—C1—C2—C3 | 0.07 |
O1vii—Fe1—N1—C1 | −137.63 | C1—C2—C3—C2viii | −0.81 |
O1viii—Fe1—N1—C1 | 132.81 | | |
Symmetry codes: (i) −x, y, −z+2; (ii) −x, y, −z+1; (iii) x−1/2, −y+1/2, z+1/2; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+1, −y, −z+1; (vi) −x+1, y, −z+1; (vii) −x, −y, −z+2; (viii) x, −y, z. |
(12)
trans-(1,4,8,11-Tetra-azacyclotetradecane)-dioxo-rhenium hexafluorophosphate
top
Crystal data top
F6P·C10H24N4O2Re | γ = 90° |
Mr = 563.49 | V = 1706.4 (6) Å3 |
Monclinic, I2/a | Z = 4 |
Hall symbol: -I 2ya | F(000) = 992 |
a = 17.257 (4) Å | Dx = 2.099 Mg m−3 |
b = 5.533 (1) Å | Mo Kα radiation, λ = 0.71070 Å |
c = 18.053 (4) Å | µ = 7.29 mm−1 |
α = 90° | T = 293 K |
β = 98.14 (2)° | × × mm |
Data collection top
Radiation source: fine-focus sealed tube | θmax = 30.1°, θmin = 2.3° |
4752 measured reflections | h = −15→24 |
2500 independent reflections | k = −7→7 |
2150 reflections with I > 2σ(I) | l = −25→16 |
Rint = 0.121 | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.077 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.192 | w = 1/[σ2(Fo2) + (0.069P)2 + 29.4858P] where P = (Fo2 + 2Fc2)/3 |
S = 1.32 | (Δ/σ)max = 0.001 |
2500 reflections | Δρmax = 5.90 e Å−3 |
129 parameters | Δρmin = −4.02 e Å−3 |
1 restraint | Extinction correction: nne |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
F6P·C10H24N4O2Re | γ = 90° |
Mr = 563.49 | V = 1706.4 (6) Å3 |
Monclinic, I2/a | Z = 4 |
a = 17.257 (4) Å | Mo Kα radiation |
b = 5.533 (1) Å | µ = 7.29 mm−1 |
c = 18.053 (4) Å | T = 293 K |
α = 90° | × × mm |
β = 98.14 (2)° | |
Data collection top
4752 measured reflections | 2150 reflections with I > 2σ(I) |
2500 independent reflections | Rint = 0.121 |
Refinement top
R[F2 > 2σ(F2)] = 0.077 | 1 restraint |
wR(F2) = 0.192 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.32 | w = 1/[σ2(Fo2) + (0.069P)2 + 29.4858P] where P = (Fo2 + 2Fc2)/3 |
2500 reflections | Δρmax = 5.90 e Å−3 |
129 parameters | Δρmin = −4.02 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is nt relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Re1 | 0.0000 | 0.0000 | 0.0000 | 0.0191 (2) | |
O1 | 0.0620 (4) | 0.2448 (13) | −0.0085 (4) | 0.0287 (13) | |
N1 | 0.0946 (4) | −0.2413 (17) | −0.0057 (4) | 0.0274 (15) | |
N2 | −0.0417 (6) | 0.0197 (14) | −0.1171 (5) | 0.0274 (18) | |
C1 | 0.1374 (6) | −0.1928 (19) | −0.0719 (5) | 0.0318 (19) | |
C2 | 0.0795 (7) | −0.203 (2) | −0.1450 (6) | 0.041 (2) | |
C3 | 0.0263 (9) | 0.022 (2) | −0.1628 (7) | 0.038 (3) | |
C4 | −0.0954 (6) | 0.2315 (19) | −0.1296 (5) | 0.034 (2) | |
C5 | 0.1472 (5) | −0.231 (2) | 0.0680 (6) | 0.036 (2) | |
P1 | 0.2500 | 0.2500 | 0.2500 | 0.0358 (8) | |
F1 | 0.268 (6) | 0.20 (3) | 0.165 (5) | 0.080* | 0.16 (4) |
F2 | 0.314 (7) | 0.39 (2) | 0.203 (5) | 0.080* | 0.14 (4) |
F3 | 0.222 (3) | 0.044 (10) | 0.302 (3) | 0.080* | 0.37 (5) |
F4 | 0.162 (2) | 0.290 (6) | 0.210 (4) | 0.080* | 0.56 (8) |
F5 | 0.238 (2) | 0.525 (7) | 0.279 (3) | 0.080* | 0.37 (4) |
F6 | 0.183 (5) | 0.270 (13) | 0.179 (5) | 0.080* | 0.19 (4) |
F7 | 0.152 (3) | 0.248 (12) | 0.233 (5) | 0.080* | 0.30 (10) |
F8 | 0.224 (6) | 0.16 (3) | 0.330 (6) | 0.080* | 0.16 (4) |
F9 | 0.229 (10) | 0.27 (2) | 0.161 (6) | 0.080* | 0.11 (3) |
F10 | 0.2610 (17) | 0.058 (9) | 0.185 (2) | 0.080* | 0.44 (4) |
F11 | 0.240 (4) | −0.051 (14) | 0.263 (4) | 0.080* | 0.22 (4) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Re1 | 0.0219 (3) | 0.0163 (3) | 0.0181 (3) | −0.00234 (13) | −0.00104 (15) | −0.00013 (13) |
O1 | 0.035 (3) | 0.019 (3) | 0.032 (3) | −0.007 (3) | 0.003 (2) | 0.005 (3) |
N1 | 0.025 (3) | 0.025 (4) | 0.031 (3) | 0.006 (3) | 0.004 (3) | 0.002 (3) |
N2 | 0.036 (4) | 0.028 (5) | 0.016 (3) | −0.003 (3) | −0.002 (3) | 0.000 (3) |
C1 | 0.038 (5) | 0.030 (5) | 0.031 (4) | −0.001 (4) | 0.016 (4) | −0.006 (4) |
C2 | 0.049 (6) | 0.040 (6) | 0.036 (5) | 0.001 (5) | 0.010 (4) | −0.010 (5) |
C3 | 0.059 (7) | 0.032 (6) | 0.024 (4) | −0.007 (4) | 0.011 (4) | −0.007 (4) |
C4 | 0.037 (4) | 0.027 (5) | 0.034 (4) | 0.006 (4) | −0.009 (4) | 0.010 (4) |
C5 | 0.030 (4) | 0.034 (5) | 0.039 (5) | 0.005 (4) | −0.015 (4) | −0.003 (4) |
P1 | 0.0372 (17) | 0.0275 (18) | 0.0380 (17) | 0.0000 (15) | −0.0104 (14) | −0.0010 (15) |
Geometric parameters (Å, º) top
Re1—O1i | 1.746 (7) | F2—F7ii | 1.43 (13) |
Re1—O1 | 1.746 (7) | F2—F11ii | 1.50 (14) |
Re1—N1i | 2.123 (8) | F2—F9 | 1.68 (18) |
Re1—N1 | 2.123 (8) | F3—F2ii | 0.73 (10) |
Re1—N2 | 2.136 (8) | F3—F8 | 0.80 (12) |
Re1—N2i | 2.136 (8) | F3—F11 | 0.96 (8) |
N1—C5 | 1.501 (11) | F3—F9ii | 1.42 (14) |
N1—C1 | 1.515 (12) | F3—F1ii | 1.52 (13) |
N2—C4 | 1.492 (13) | F3—F5ii | 1.73 (8) |
N2—C3 | 1.528 (17) | F4—F7 | 0.52 (6) |
C1—C2 | 1.540 (15) | F4—F6 | 0.73 (9) |
C2—C3 | 1.552 (18) | F4—F9 | 1.56 (16) |
C4—C5i | 1.522 (16) | F5—F10ii | 0.79 (5) |
C5—C4i | 1.522 (16) | F5—F11ii | 0.89 (7) |
P1—F3ii | 1.59 (4) | F5—F1ii | 1.63 (14) |
P1—F3 | 1.59 (4) | F5—F3ii | 1.73 (8) |
P1—F4 | 1.60 (2) | F6—F9 | 0.89 (14) |
P1—F4ii | 1.60 (3) | F6—F7 | 1.19 (12) |
P1—F6ii | 1.60 (6) | F6—F8ii | 1.68 (13) |
P1—F6 | 1.60 (6) | F6—F10 | 1.77 (10) |
P1—F9ii | 1.60 (10) | F7—F2ii | 1.43 (13) |
P1—F9 | 1.60 (10) | F8—F1ii | 0.80 (13) |
P1—F10ii | 1.61 (4) | F8—F2ii | 0.85 (13) |
P1—F10 | 1.61 (4) | F8—F9ii | 0.90 (16) |
P1—F1ii | 1.62 (8) | F8—F10ii | 1.64 (14) |
P1—F1 | 1.62 (8) | F8—F6ii | 1.68 (13) |
F1—F9 | 0.77 (14) | F8—F11 | 1.71 (15) |
F1—F8ii | 0.80 (13) | F9—F8ii | 0.90 (16) |
F1—F10 | 0.89 (13) | F9—F10 | 1.37 (14) |
F1—F2 | 1.41 (17) | F9—F3ii | 1.42 (14) |
F1—F3ii | 1.52 (13) | F10—F5ii | 0.79 (5) |
F1—F6 | 1.55 (14) | F10—F11 | 1.61 (8) |
F1—F5ii | 1.63 (14) | F10—F8ii | 1.64 (14) |
F2—F3ii | 0.73 (10) | F11—F5ii | 0.89 (7) |
F2—F8ii | 0.85 (13) | F11—F2ii | 1.50 (14) |
| | | |
O1i—Re1—O1 | 180.0 (6) | F11—F3—F1ii | 139 (7) |
O1i—Re1—N1i | 89.9 (4) | F9ii—F3—F1ii | 30 (5) |
O1—Re1—N1i | 90.1 (4) | F2ii—F3—P1 | 83 (8) |
O1i—Re1—N1 | 90.1 (4) | F8—F3—P1 | 80 (7) |
O1—Re1—N1 | 89.9 (4) | F11—F3—P1 | 79 (6) |
N1i—Re1—N1 | 180.0 (5) | F9ii—F3—P1 | 64 (5) |
O1i—Re1—N2 | 90.1 (3) | F1ii—F3—P1 | 63 (4) |
O1—Re1—N2 | 89.9 (3) | F2ii—F3—F5ii | 117 (10) |
N1i—Re1—N2 | 82.1 (3) | F8—F3—F5ii | 136 (8) |
N1—Re1—N2 | 97.9 (3) | F11—F3—F5ii | 20 (5) |
O1i—Re1—N2i | 89.9 (3) | F9ii—F3—F5ii | 106 (7) |
O1—Re1—N2i | 90.1 (3) | F1ii—F3—F5ii | 119 (5) |
N1i—Re1—N2i | 97.9 (3) | P1—F3—F5ii | 59 (2) |
N1—Re1—N2i | 82.1 (3) | F7—F4—F6 | 144 (10) |
N2—Re1—N2i | 180.0 (6) | F7—F4—F9 | 141 (9) |
C5—N1—C1 | 113.0 (7) | F6—F4—F9 | 18 (7) |
C5—N1—Re1 | 107.8 (6) | F7—F4—P1 | 89 (7) |
C1—N1—Re1 | 113.0 (6) | F6—F4—P1 | 77 (6) |
C4—N2—C3 | 114.8 (8) | F9—F4—P1 | 61 (5) |
C4—N2—Re1 | 107.8 (6) | F10ii—F5—F11ii | 145 (8) |
C3—N2—Re1 | 111.0 (7) | F10ii—F5—P1 | 75 (4) |
N1—C1—C2 | 109.9 (8) | F11ii—F5—P1 | 78 (6) |
C1—C2—C3 | 116.2 (9) | F10ii—F5—F1ii | 16 (5) |
N2—C3—C2 | 110.9 (9) | F11ii—F5—F1ii | 136 (7) |
N2—C4—C5i | 107.8 (8) | P1—F5—F1ii | 60 (4) |
N1—C5—C4i | 107.7 (7) | F10ii—F5—F3ii | 127 (5) |
F3ii—P1—F3 | 180 (4) | F11ii—F5—F3ii | 22 (6) |
F3ii—P1—F4 | 89 (3) | P1—F5—F3ii | 57 (2) |
F3—P1—F4 | 91 (3) | F1ii—F5—F3ii | 115 (4) |
F3ii—P1—F4ii | 91 (3) | F4—F6—F9 | 148 (10) |
F3—P1—F4ii | 89 (3) | F4—F6—F7 | 15 (5) |
F4—P1—F4ii | 180 (4) | F9—F6—F7 | 146 (10) |
F3ii—P1—F6ii | 106 (4) | F4—F6—F1 | 138 (8) |
F3—P1—F6ii | 74 (4) | F9—F6—F1 | 19 (10) |
F4—P1—F6ii | 154 (3) | F7—F6—F1 | 130 (6) |
F4ii—P1—F6ii | 26 (3) | F4—F6—P1 | 77 (6) |
F3ii—P1—F6 | 74 (4) | F9—F6—P1 | 74 (8) |
F3—P1—F6 | 106 (4) | F7—F6—P1 | 72 (4) |
F4—P1—F6 | 26 (3) | F1—F6—P1 | 62 (4) |
F4ii—P1—F6 | 154 (3) | F4—F6—F8ii | 129 (9) |
F6ii—P1—F6 | 180.000 (11) | F9—F6—F8ii | 20 (9) |
F3ii—P1—F9ii | 127 (5) | F7—F6—F8ii | 131 (6) |
F3—P1—F9ii | 53 (5) | F1—F6—F8ii | 28 (5) |
F4—P1—F9ii | 122 (6) | P1—F6—F8ii | 61 (4) |
F4ii—P1—F9ii | 58 (6) | F4—F6—F10 | 120 (8) |
F6ii—P1—F9ii | 32 (5) | F9—F6—F10 | 49 (10) |
F6—P1—F9ii | 148 (5) | F7—F6—F10 | 108 (5) |
F3ii—P1—F9 | 53 (5) | F1—F6—F10 | 30 (5) |
F3—P1—F9 | 127 (5) | P1—F6—F10 | 57 (3) |
F4—P1—F9 | 58 (6) | F8ii—F6—F10 | 57 (5) |
F4ii—P1—F9 | 122 (6) | F4—F7—F6 | 21 (7) |
F6ii—P1—F9 | 148 (5) | F4—F7—F2ii | 137 (9) |
F6—P1—F9 | 32 (5) | F6—F7—F2ii | 123 (6) |
F9ii—P1—F9 | 180.000 (12) | F4—F7—P1 | 73 (7) |
F3ii—P1—F10ii | 92 (3) | F6—F7—P1 | 65 (4) |
F3—P1—F10ii | 88 (3) | F2ii—F7—P1 | 64 (5) |
F4—P1—F10ii | 92 (2) | F3—F8—F1ii | 145 (10) |
F4ii—P1—F10ii | 88 (2) | F3—F8—F2ii | 52 (10) |
F6ii—P1—F10ii | 67 (4) | F1ii—F8—F2ii | 117 (10) |
F6—P1—F10ii | 113 (4) | F3—F8—F9ii | 114 (10) |
F9ii—P1—F10ii | 50 (5) | F1ii—F8—F9ii | 54 (10) |
F9—P1—F10ii | 130 (5) | F2ii—F8—F9ii | 147 (10) |
F3ii—P1—F10 | 88 (3) | F3—F8—F10ii | 129 (9) |
F3—P1—F10 | 92 (3) | F1ii—F8—F10ii | 16 (8) |
F4—P1—F10 | 88 (2) | F2ii—F8—F10ii | 106 (10) |
F4ii—P1—F10 | 92 (2) | F9ii—F8—F10ii | 56 (10) |
F6ii—P1—F10 | 113 (4) | F3—F8—P1 | 71 (7) |
F6—P1—F10 | 67 (4) | F1ii—F8—P1 | 73 (9) |
F9ii—P1—F10 | 130 (5) | F2ii—F8—P1 | 76 (9) |
F9—P1—F10 | 50 (5) | F9ii—F8—P1 | 71 (9) |
F10ii—P1—F10 | 180 (2) | F10ii—F8—P1 | 59 (3) |
F3ii—P1—F1ii | 123 (5) | F3—F8—F6ii | 95 (9) |
F3—P1—F1ii | 57 (5) | F1ii—F8—F6ii | 67 (10) |
F4—P1—F1ii | 96 (4) | F2ii—F8—F6ii | 131 (10) |
F4ii—P1—F1ii | 84 (4) | F9ii—F8—F6ii | 20 (9) |
F6ii—P1—F1ii | 58 (5) | F10ii—F8—F6ii | 65 (5) |
F6—P1—F1ii | 122 (5) | P1—F8—F6ii | 57 (4) |
F9ii—P1—F1ii | 28 (5) | F3—F8—F11 | 14 (6) |
F9—P1—F1ii | 152 (5) | F1ii—F8—F11 | 133 (10) |
F10ii—P1—F1ii | 32 (5) | F2ii—F8—F11 | 61 (10) |
F10—P1—F1ii | 148 (5) | F9ii—F8—F11 | 101 (10) |
F3ii—P1—F1 | 57 (5) | F10ii—F8—F11 | 119 (5) |
F3—P1—F1 | 123 (5) | P1—F8—F11 | 60 (4) |
F4—P1—F1 | 84 (4) | F6ii—F8—F11 | 81 (6) |
F4ii—P1—F1 | 96 (4) | F1—F9—F6 | 138 (10) |
F6ii—P1—F1 | 122 (5) | F1—F9—F8ii | 57 (10) |
F6—P1—F1 | 58 (5) | F6—F9—F8ii | 140 (10) |
F9ii—P1—F1 | 152 (5) | F1—F9—F10 | 38 (10) |
F9—P1—F1 | 28 (5) | F6—F9—F10 | 101 (10) |
F10ii—P1—F1 | 148 (5) | F8ii—F9—F10 | 91 (10) |
F10—P1—F1 | 32 (5) | F1—F9—F3ii | 82 (10) |
F1ii—P1—F1 | 180.0 (15) | F6—F9—F3ii | 110 (10) |
F9—F1—F8ii | 70 (10) | F8ii—F9—F3ii | 31 (9) |
F9—F1—F10 | 110 (10) | F10—F9—F3ii | 106 (10) |
F8ii—F1—F10 | 151 (10) | F1—F9—F4 | 132 (10) |
F9—F1—F2 | 96 (10) | F6—F9—F4 | 14 (6) |
F8ii—F1—F2 | 33 (9) | F8ii—F9—F4 | 127 (10) |
F10—F1—F2 | 124 (10) | F10—F9—F4 | 99 (8) |
F9—F1—F3ii | 68 (10) | F3ii—F9—F4 | 97 (7) |
F8ii—F1—F3ii | 18 (8) | F1—F9—P1 | 77 (10) |
F10—F1—F3ii | 133 (8) | F6—F9—P1 | 74 (8) |
F2—F1—F3ii | 28 (5) | F8ii—F9—P1 | 77 (9) |
F9—F1—F6 | 23 (10) | F10—F9—P1 | 65 (5) |
F8ii—F1—F6 | 85 (10) | F3ii—F9—P1 | 63 (5) |
F10—F1—F6 | 89 (8) | F4—F9—P1 | 61 (4) |
F2—F1—F6 | 104 (9) | F1—F9—F2 | 57 (10) |
F3ii—F1—F6 | 77 (6) | F6—F9—F2 | 127 (10) |
F9—F1—P1 | 75 (10) | F8ii—F9—F2 | 16 (7) |
F8ii—F1—P1 | 78 (10) | F10—F9—F2 | 84 (9) |
F10—F1—P1 | 73 (6) | F3ii—F9—F2 | 26 (4) |
F2—F1—P1 | 66 (5) | F4—F9—F2 | 113 (7) |
F3ii—F1—P1 | 61 (4) | P1—F9—F2 | 61 (5) |
F6—F1—P1 | 61 (4) | F5ii—F10—F1 | 149 (9) |
F9—F1—F5ii | 109 (10) | F5ii—F10—F9 | 137 (8) |
F8ii—F1—F5ii | 136 (10) | F1—F10—F9 | 32 (8) |
F10—F1—F5ii | 15 (4) | F5ii—F10—F11 | 18 (4) |
F2—F1—F5ii | 110 (7) | F1—F10—F11 | 138 (7) |
F3ii—F1—F5ii | 119 (5) | F9—F10—F11 | 119 (7) |
F6—F1—F5ii | 87 (6) | F5ii—F10—P1 | 77 (4) |
P1—F1—F5ii | 60 (4) | F1—F10—P1 | 74 (7) |
F3ii—F2—F8ii | 60 (10) | F9—F10—P1 | 65 (5) |
F3ii—F2—F1 | 85 (10) | F11—F10—P1 | 63 (3) |
F8ii—F2—F1 | 30 (10) | F5ii—F10—F8ii | 135 (7) |
F3ii—F2—F7ii | 128 (10) | F1—F10—F8ii | 14 (7) |
F8ii—F2—F7ii | 127 (10) | F9—F10—F8ii | 33 (6) |
F1—F2—F7ii | 99 (8) | F11—F10—F8ii | 125 (5) |
F3ii—F2—F11ii | 32 (8) | P1—F10—F8ii | 61 (4) |
F8ii—F2—F11ii | 89 (10) | F5ii—F10—F6 | 111 (6) |
F1—F2—F11ii | 107 (9) | F1—F10—F6 | 61 (7) |
F7ii—F2—F11ii | 101 (6) | F9—F10—F6 | 30 (6) |
F3ii—F2—P1 | 71 (8) | F11—F10—F6 | 93 (4) |
F8ii—F2—P1 | 74 (9) | P1—F10—F6 | 56 (3) |
F1—F2—P1 | 63 (5) | F8ii—F10—F6 | 59 (4) |
F7ii—F2—P1 | 65 (5) | F5ii—F11—F3 | 138 (10) |
F11ii—F2—P1 | 64 (5) | F5ii—F11—F2ii | 127 (8) |
F3ii—F2—F9 | 57 (10) | F3—F11—F2ii | 24 (5) |
F8ii—F2—F9 | 17 (8) | F5ii—F11—F10 | 16 (4) |
F1—F2—F9 | 27 (5) | F3—F11—F10 | 125 (7) |
F7ii—F2—F9 | 114 (7) | F2ii—F11—F10 | 111 (6) |
F11ii—F2—F9 | 81 (8) | F5ii—F11—P1 | 71 (6) |
P1—F2—F9 | 57 (5) | F3—F11—P1 | 67 (5) |
F2ii—F3—F8 | 68 (9) | F2ii—F11—P1 | 63 (4) |
F2ii—F3—F11 | 125 (10) | F10—F11—P1 | 58 (3) |
F8—F3—F11 | 154 (10) | F5ii—F11—F8 | 128 (8) |
F2ii—F3—F9ii | 97 (10) | F3—F11—F8 | 12 (5) |
F8—F3—F9ii | 35 (9) | F2ii—F11—F8 | 30 (4) |
F11—F3—F9ii | 120 (9) | F10—F11—F8 | 117 (5) |
F2ii—F3—F1ii | 67 (10) | P1—F11—F8 | 58 (4) |
F8—F3—F1ii | 18 (8) | | |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1/2, −y+1/2, −z+1/2. |
(13) bis(mu!4$-
N,
N-Diethylcarbamato-
O,
O',
O'',
O''')-tetrakis(mu!3$-
N,
N-diethylcarba- mato-
O,
O',
O'')-hexakis(mu!2$-
N,
N-diethylcarbamato-O,
O')-hexa-iron
top
Crystal data top
C60H120Fe6N12O24 | Z = 4 |
Mr = 1728.78 | F(000) = 3168 |
Orthorhombic, Ccca | Dx = 1.259 Mg m−3 |
Hall symbol: -C 2b 2bc | Mo K\a radiation, λ = 0.71073 Å |
a = 20.939 (2) Å | µ = 1.07 mm−1 |
b = 25.243 (4) Å | T = 0 K |
c = 16.048 (1) Å | × × mm |
V = 8482.4 (17) Å3 | |
Crystal data top
C60H120Fe6N12O24 | V = 8482.4 (17) Å3 |
Mr = 1728.78 | Z = 4 |
Orthorhombic, Ccca | Mo K\a radiation |
a = 20.939 (2) Å | µ = 1.07 mm−1 |
b = 25.243 (4) Å | T = 0 K |
c = 16.048 (1) Å | × × mm |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe1 | 0.13156 | 0.20392 | 0.32463 | 0.02* | |
Fe3 | 0 | 0.16095 | 0.25 | 0.02* | |
O1 | 0.223 | 0.21055 | 0.28235 | 0.02* | |
O3 | 0.12755 | 0.1322 | 0.3766 | 0.02* | |
O4 | 0.1412 | 0.27105 | 0.39045 | 0.02* | |
O7 | 0.0987 | 0.17740 | 0.20855 | 0.02* | |
O9 | 0.02975 | 0.2134 | 0.34335 | 0.02* | |
O10 | 0.03490 | 0.10065 | 0.3225 | 0.02* | |
N1 | 0.09530 | 0.04935 | 0.4043 | 0.02* | |
N2 | 0.1485 | 0.35895 | 0.4016 | 0.02* | |
N3 | 0 | 0.25 | 0.4663 | 0.02* | |
N6 | 0.3149 | 0.25 | 0.25 | 0.02* | |
C1 | 0.0855 | 0.09645 | 0.36540 | 0.02* | |
C2 | 0.04775 | 0.00445 | 0.3956 | 0.02* | |
C3 | 0.0694 | −0.02960 | 0.3245 | 0.02* | |
C4 | 0.15315 | 0.04035 | 0.4533 | 0.02* | |
C5 | 0.1394 | 0.05275 | 0.542 | 0.02* | |
C6 | 0.12945 | 0.316 | 0.36135 | 0.02* | |
C7 | 0.1854 | 0.3527 | 0.4801 | 0.02* | |
C8 | 0.1381 | 0.4124 | 0.37035 | 0.02* | |
C9 | 0.19365 | 0.4314 | 0.3148 | 0.02* | |
C10 | 0.25335 | 0.3314 | 0.466 | 0.02* | |
C11 | 0 | 0.25 | 0.3825 | 0.02* | |
C12 | 0.03335 | 0.20945 | 0.51325 | 0.02* | |
C13 | −0.00605 | 0.16165 | 0.53225 | 0.02* | |
C26 | 0.2503 | 0.25 | 0.25 | 0.02* | |
C27 | 0.35015 | 0.2089 | 0.29265 | 0.02* | |
C28 | 0.36645 | 0.1639 | 0.2335 | 0.02* | |
Geometric parameters (Å, º) top
Fe1—O1 | 2.0382 | N1—C2 | 1.5151 |
Fe1—O3 | 1.9951 | N1—C4 | 1.4619 |
Fe1—O4 | 2.007 | N2—C6 | 1.3236 |
Fe1—O7 | 2.0957 | N2—C7 | 1.4862 |
Fe1—O9 | 2.1661 | N2—C8 | 1.4558 |
Fe3—O7 | 2.2104 | N3—C11 | 1.3448 (2) |
Fe3—O9 | 2.0941 | N3—C12 | 1.4502 |
Fe3—O10 | 2.0505 | N6—C26 | 1.3527 (2) |
O1—C26 | 1.2601 | N6—C27 | 1.4456 |
O3—C1 | 1.2736 | C2—C3 | 1.4987 |
O4—C6 | 1.2514 | C4—C5 | 1.4856 |
O7—C6i | 1.3041 | C7—C10 | 1.5377 |
O9—C11 | 1.2792 | C8—C9 | 1.542 |
O10—C1 | 1.268 | C12—C13 | 1.4932 |
N1—C1 | 1.3585 | C27—C28 | 1.5192 |
| | | |
Fe1···C12 | 3.6621 | C3···O10 | 3.3665 |
Fe1···Fe1i | 3.3391 | C5···O3 | 3.3361 |
Fe3···C8ii | 3.9396 | C6···C11 | 3.1997 |
Fe3···C8i | 3.9396 | C6···C26 | 3.5174 |
O1···C28 | 3.3202 | C8···Fe3ii | 3.9396 |
O3···C5 | 3.3361 | C8···Fe3ii | 3.9396 |
O4···N3 | 3.2412 | C9···O7i | 3.4112 |
O4···C10 | 3.0505 | C10···O4 | 3.0505 |
O4···C12 | 3.3766 | C11···C6 | 3.1997 |
O7···O9i | 3.2213 | C11···C6ii | 3.1997 |
O7···C9i | 3.4112 | C12···Fe1 | 3.6621 |
O9···C13 | 3.385 | C12···O4 | 3.3766 |
O9···O7i | 3.2213 | C13···O9 | 3.385 |
O10···C3 | 3.3665 | C26···C6 | 3.5174 |
N3···O4 | 3.2412 | C26···C6i | 3.5174 |
N3···O4ii | 3.2412 | C28···O1 | 3.3202 |
| | | |
O1—Fe1—O3 | 104.67 | Fe3—O9—C11 | 131.54 |
O1—Fe1—O4 | 90.65 | Fe3—O10—C1 | 131.91 |
O1—Fe1—O7 | 92.22 | C1—N1—C2 | 120.87 |
O1—Fe1—O9 | 164.07 | C1—N1—C4 | 120.55 |
O3—Fe1—O4 | 123.4 | C2—N1—C4 | 118.54 |
O3—Fe1—O7 | 93.89 | C6—N2—C7 | 118.91 |
O3—Fe1—O9 | 90.05 | C6—N2—C8 | 123.09 |
O4—Fe1—O7 | 140.41 | C7—N2—C8 | 117.91 |
O4—Fe1—O9 | 86.14 | C11—N3—C12 | 121.3 |
O7—Fe1—O9 | 80.53 | C11—N3—C12ii | 121.3 |
O7—Fe3—O9 | 79.54 | C12—N3—C12ii | 117.4 |
O7—Fe3—O10 | 88.68 | C26—N6—C27 | 120.7 |
O7—Fe3—O7iii | 158.34 | C26—N6—C27i | 120.7 |
O7—Fe3—O9iii | 86.79 | C27—N6—C27i | 118.59 |
O7—Fe3—O10iii | 107.57 | O3—C1—O10 | 126.52 |
O9—Fe3—O10 | 87.56 | O3—C1—N1 | 116.8 |
O7iii—Fe3—O9 | 86.79 | O10—C1—N1 | 116.67 |
O9—Fe3—O9iii | 101.57 | N1—C2—C3 | 107.48 |
O9—Fe3—O10iii | 168.89 | N1—C4—C5 | 108.79 |
O7iii—Fe3—O10 | 107.57 | O4—C6—N2 | 120.09 |
O9iii—Fe3—O10 | 168.89 | O4—C6—O7i | 122.27 |
O10—Fe3—O10iii | 84.14 | O7i—C6—N2 | 117.64 |
O7iii—Fe3—O9iii | 79.54 | N2—C7—C10 | 113.17 |
O7iii—Fe3—O10iii | 88.68 | N2—C8—C9 | 112 |
O9iii—Fe3—O10iii | 87.56 | O9—C11—N3 | 119.42 |
Fe1—O1—C26 | 128.91 | O9—C11—O9ii | 121.17 |
Fe1—O3—C1 | 127.82 | O9ii—C11—N3 | 119.42 |
Fe1—O4—C6 | 123.32 | N3—C12—C13 | 114.23 |
Fe1—O7—Fe3 | 95.71 | O1—C26—N6 | 116.98 |
Fe1—O7—C6i | 124.17 | O1—C26—O1i | 126.05 |
Fe3—O7—C6i | 138.11 | O1i—C26—N6 | 116.98 |
Fe1—O9—Fe3 | 97.11 | N6—C27—C28 | 110.83 |
Fe1—O9—C11 | 128.84 | | |
| | | |
O3—Fe1—O1—C26 | −174.59 | O7iii—Fe3—O10—C1 | −127.50 |
O4—Fe1—O1—C26 | −49.70 | O10iii—Fe3—O10—C1 | 145.75 |
O7—Fe1—O1—C26 | 90.8 | Fe1—O1—C26—O1i | −19.30 |
O1—Fe1—O3—C1 | −131.40 | Fe1—O1—C26—N6 | 160.7 |
O4—Fe1—O3—C1 | 127.84 | Fe1—O3—C1—N1 | 176.13 |
O7—Fe1—O3—C1 | −38.08 | Fe1—O3—C1—O10 | −4.95 |
O9—Fe1—O3—C1 | 42.43 | Fe1—O4—C6—N2 | −166.62 |
O1—Fe1—O4—C6 | 88.61 | Fe1—O4—C6—O7i | 13.22 |
O3—Fe1—O4—C6 | −163.28 | Fe1i—O7i—C6—N2 | 117.28 |
O7—Fe1—O4—C6 | −5.67 | Fe1i—O7i—C6—O4 | −62.56 |
O9—Fe1—O4—C6 | −75.77 | Fe3—O9—C11—N3 | 126.7 |
O1—Fe1—O7—Fe3 | 174.7 | Fe1—O9—C11—N3 | −75.55 |
O1—Fe1—O7—C6i | −18.84 | Fe3—O9—C11—O9ii | −53.30 |
O3—Fe1—O7—Fe3 | 69.83 | Fe1—O9—C11—O9ii | 104.45 |
O3—Fe1—O7—C6i | −123.71 | Fe3—O10—C1—O3 | 3.48 |
O4—Fe1—O7—Fe3 | −91.59 | Fe3—O10—C1—N1 | −177.59 |
O4—Fe1—O7—C6i | 74.87 | C1—N1—C2—C3 | 93.05 |
O9—Fe1—O7—Fe3 | −19.57 | C4—N1—C2—C3 | −84.95 |
O9—Fe1—O7—C6i | 146.89 | C4—N1—C1—O10 | 178.34 |
O3—Fe1—O9—Fe3 | −73.17 | C2—N1—C1—O10 | 0.38 |
O3—Fe1—O9—C11 | 123.43 | C2—N1—C1—O3 | 179.42 |
O4—Fe1—O9—Fe3 | 163.35 | C1—N1—C4—C5 | 94.43 |
O4—Fe1—O9—C11 | −0.06 | C4—N1—C1—O3 | −2.62 |
O7—Fe1—O9—Fe3 | 20.77 | C2—N1—C4—C5 | −87.57 |
O7—Fe1—O9—C11 | −142.64 | C7—N2—C6—O7i | −178.14 |
O9—Fe3—O7—Fe1 | 20.34 | C7—N2—C6—O4 | 1.71 |
O9—Fe3—O7—C6i | −142.79 | C8—N2—C6—O4 | 178.23 |
O10—Fe3—O7—Fe1 | −67.42 | C6—N2—C8—C9 | −89.66 |
O10—Fe3—O7—C6i | 129.45 | C7—N2—C8—C9 | 86.89 |
O7iii—Fe3—O7—Fe1 | 72.08 | C8—N2—C7—C10 | −106.27 |
O9iii—Fe3—O7—Fe1 | 122.73 | C6—N2—C7—C10 | 70.43 |
O10iii—Fe3—O7—Fe1 | −150.85 | C8—N2—C6—O7i | −1.62 |
O7—Fe3—O9—Fe1 | −19.71 | C12ii—N3—C11—O9 | −179.69 |
O7—Fe3—O9—C11 | 143 | C12—N3—C11—O9 | 0.31 |
O10—Fe3—O9—Fe1 | 69.4 | C12ii—N3—C12—C13 | 90.66 |
O10—Fe3—O9—C11 | −127.89 | C12—N3—C11—O9ii | −179.69 |
O7iii—Fe3—O9—Fe1 | 177.16 | C11—N3—C12—C13 | −89.34 |
O7iii—Fe3—O9—C11 | −20.13 | C27—N6—C26—O1 | −5.88 |
O9iii—Fe3—O9—Fe1 | −104.21 | C27i—N6—C26—O1 | 174.12 |
O9iii—Fe3—O9—C11 | 58.5 | C27—N6—C26—O1i | 174.12 |
O7—Fe3—O10—C1 | 37.94 | C26—N6—C27—C28 | 93.08 |
O9—Fe3—O10—C1 | −41.64 | C27i—N6—C27—C28 | −86.92 |
Symmetry codes: (i) x, −y+1/2, −z+1/2; (ii) −x, −y+1/2, z; (iii) −x, y, −z+1/2. |
(14) bis(2,2'-bis(
p-tolylphosphin)-1,1-binaphthyl)-palladium(0) benzene solvate
top
Crystal data top
C96H80P4Pd·4(C6H6) | Z = 4 |
Mr = 1776.33 | F(000) = 3304 |
Orthorhombic, C2221 | Dx = 1.162 Mg m−3 |
Hall symbol: C 2c 2 | Mo K\a radiation, λ = 0.71073 Å |
a = 29.327 (12) Å | µ = 0.31 mm−1 |
b = 16.743 (7) Å | T = 0 K |
c = 19.458 (6) Å | × × mm |
V = 9554 (6) Å3 | |
Refinement top
0 restraints | |
See text | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
Crystal data top
C96H80P4Pd·4(C6H6) | V = 9554 (6) Å3 |
Mr = 1776.33 | Z = 4 |
Orthorhombic, C2221 | Mo K\a radiation |
a = 29.327 (12) Å | µ = 0.31 mm−1 |
b = 16.743 (7) Å | T = 0 K |
c = 19.458 (6) Å | × × mm |
Refinement top
0 restraints | Absolute structure: Flack H.D. (1983), Acta Cryst. A39, 876-881 |
See text | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pd1 | 0 | 0.26357 | 0.25 | 0.02* | |
P1 | 0.06025 | 0.1953 | 0.30795 | 0.02* | |
P2 | 0.05415 | 0.335 | 0.18055 | 0.02* | |
C1 | 0.08672 | 0.25043 | 0.37955 | 0.02* | |
C2 | 0.06225 | 0.31235 | 0.4078 | 0.02* | |
C3 | 0.07878 | 0.35642 | 0.4636 | 0.02* | |
C4 | 0.12003 | 0.33983 | 0.49265 | 0.02* | |
C5 | 0.14548 | 0.27772 | 0.46425 | 0.02* | |
C6 | 0.1294 | 0.2334 | 0.4082 | 0.02* | |
C7 | 0.1374 | 0.3865 | 0.55415 | 0.02* | |
C8 | 0.05257 | 0.09622 | 0.34795 | 0.02* | |
C9 | 0.01047 | 0.05807 | 0.34415 | 0.02* | |
C10 | 0.00405 | −0.01695 | 0.37475 | 0.02* | |
C11 | 0.03985 | −0.05500 | 0.4095 | 0.02* | |
C12 | 0.08078 | −0.01708 | 0.41295 | 0.02* | |
C13 | 0.08748 | 0.05748 | 0.38315 | 0.02* | |
C14 | 0.03385 | −0.13470 | 0.44435 | 0.02* | |
C15 | 0.10742 | 0.17003 | 0.248 | 0.02* | |
C16 | 0.10817 | 0.09153 | 0.22185 | 0.02* | |
C17 | 0.13795 | 0.06980 | 0.1715 | 0.02* | |
C18 | 0.17088 | 0.12427 | 0.14515 | 0.02* | |
C19 | 0.20207 | 0.10302 | 0.09175 | 0.02* | |
C20 | 0.23345 | 0.15585 | 0.06725 | 0.02* | |
C21 | 0.23485 | 0.2336 | 0.0963 | 0.02* | |
C22 | 0.20470 | 0.25530 | 0.1464 | 0.02* | |
C23 | 0.17133 | 0.20207 | 0.173 | 0.02* | |
C24 | 0.13925 | 0.2253 | 0.2248 | 0.02* | |
C25 | 0.13968 | 0.31042 | 0.24985 | 0.02* | |
C26 | 0.17623 | 0.33528 | 0.2917 | 0.02* | |
C27 | 0.21285 | 0.28395 | 0.31195 | 0.02* | |
C28 | 0.24745 | 0.3103 | 0.3533 | 0.02* | |
C29 | 0.2478 | 0.38935 | 0.37835 | 0.02* | |
C30 | 0.21295 | 0.44015 | 0.3611 | 0.02* | |
C31 | 0.17677 | 0.41532 | 0.31855 | 0.02* | |
C32 | 0.1406 | 0.46695 | 0.3007 | 0.02* | |
C33 | 0.10728 | 0.44228 | 0.2579 | 0.02* | |
C34 | 0.10547 | 0.36283 | 0.23135 | 0.02* | |
C35 | 0.07718 | 0.28223 | 0.1048 | 0.02* | |
C36 | 0.05673 | 0.21072 | 0.08665 | 0.02* | |
C37 | 0.07147 | 0.16602 | 0.03145 | 0.02* | |
C38 | 0.10647 | 0.19218 | −0.00765 | 0.02* | |
C39 | 0.12797 | 0.26237 | 0.0093 | 0.02* | |
C40 | 0.1139 | 0.3064 | 0.0663 | 0.02* | |
C41 | 0.12292 | 0.14247 | −0.06965 | 0.02* | |
C42 | 0.04040 | 0.43325 | 0.14215 | 0.02* | |
C43 | −0.00062 | 0.46797 | 0.15890 | 0.02* | |
C44 | −0.01143 | 0.54488 | 0.13675 | 0.02* | |
C45 | 0.01795 | 0.5886 | 0.09905 | 0.02* | |
C46 | 0.05743 | 0.55413 | 0.08175 | 0.02* | |
C47 | 0.06915 | 0.48005 | 0.1047 | 0.02* | |
C48 | 0.0076 | 0.6748 | 0.0784 | 0.02* | |
C97 | 0.38575 | 0.18825 | 0.2585 | 0.02* | |
C98 | 0.34575 | 0.21875 | 0.245 | 0.02* | |
C99 | 0.34425 | 0.28875 | 0.226 | 0.02* | |
C100 | 0.37925 | 0.33925 | 0.223 | 0.02* | |
C101 | 0.42025 | 0.31525 | 0.2357 | 0.02* | |
C102 | 0.4225 | 0.23 | 0.2545 | 0.02* | |
C103 | 0.26525 | 0.08575 | 0.4415 | 0.02* | |
C104 | 0.29750 | 0.0585 | 0.4105 | 0.02* | |
C105 | 0.293 | 0.019 | 0.35750 | 0.02* | |
C106 | 0.25225 | 0.00975 | 0.32750 | 0.02* | |
C107 | 0.22 | 0.036 | 0.3655 | 0.02* | |
C108 | 0.22775 | 0.07825 | 0.425 | 0.02* | |
Geometric parameters (Å, º) top
Pd1—P1 | 2.3875 | C26—C27 | 1.4308 |
Pd1—P2 | 2.4038 | C26—C31 | 1.4384 |
P1—C1 | 1.8427 | C27—C28 | 1.3681 |
P1—C8 | 1.8462 | C28—C29 | 1.4105 |
P1—C15 | 1.8583 | C29—C30 | 1.3714 |
P2—C34 | 1.8599 | C30—C31 | 1.4086 |
P2—C35 | 1.8464 | C31—C32 | 1.4118 |
P2—C42 | 1.8512 | C32—C33 | 1.3487 |
C1—C2 | 1.3755 | C33—C34 | 1.428 |
C1—C6 | 1.3996 | C35—C36 | 1.3849 |
C2—C3 | 1.3994 | C35—C40 | 1.3728 |
C3—C4 | 1.3639 | C36—C37 | 1.3786 |
C4—C5 | 1.3942 | C37—C38 | 1.3507 |
C4—C7 | 1.5173 | C38—C39 | 1.3738 |
C5—C6 | 1.4009 | C38—C41 | 1.543 |
C8—C9 | 1.3921 | C39—C40 | 1.3942 |
C8—C13 | 1.3921 | C42—C43 | 1.3753 |
C9—C10 | 1.4027 | C42—C47 | 1.3623 |
C10—C11 | 1.4019 | C43—C44 | 1.3944 |
C11—C12 | 1.3596 | C44—C45 | 1.3477 |
C11—C14 | 1.5071 | C45—C46 | 1.3368 |
C12—C13 | 1.3904 | C45—C48 | 1.5286 |
C15—C16 | 1.4096 | C46—C47 | 1.3623 |
C15—C24 | 1.3898 | C97—C98 | 1.3061 |
C16—C17 | 1.362 | C97—C102 | 1.287 |
C17—C18 | 1.4238 | C98—C99 | 1.2297 |
C18—C19 | 1.4293 | C99—C100 | 1.3311 |
C18—C23 | 1.4109 | C100—C101 | 1.2916 |
C19—C20 | 1.3626 | C101—C102 | 1.4749 |
C20—C21 | 1.4198 | C103—C104 | 1.211 |
C21—C22 | 1.3653 | C103—C108 | 1.1525 |
C22—C23 | 1.4212 | C104—C105 | 1.2322 |
C23—C24 | 1.4326 | C105—C106 | 1.339 |
C24—C25 | 1.5063 | C106—C107 | 1.2784 |
C25—C26 | 1.409 | C107—C108 | 1.3757 |
C25—C34 | 1.3806 | | |
| | | |
C1···C25 | 3.1289 | C25···C1 | 3.1289 |
C1···C26 | 3.4396 | C25···C6 | 3.3537 |
C1···C34 | 3.4871 | C26···C1 | 3.4396 |
C2···C43i | 3.4264 | C26···C6 | 3.1519 |
C3···C48ii | 3.4177 | C26···C22 | 3.2378 |
C5···C27 | 3.5632 | C27···C5 | 3.5632 |
C6···C13 | 3.2287 | C27···C6 | 3.1958 |
C6···C24 | 3.5828 | C27···C22 | 3.2656 |
C6···C25 | 3.3537 | C27···C23 | 3.2668 |
C6···C26 | 3.1519 | C33···C47 | 3.246 |
C6···C27 | 3.1958 | C33···C43i | 3.5483 |
C9···C36i | 3.497 | C34···C1 | 3.4871 |
C12···C12iii | 3.4356 | C35···C15 | 3.4756 |
C13···C6 | 3.2287 | C35···C23 | 3.3446 |
C13···C16 | 3.2471 | C35···C24 | 3.1103 |
C14···C37iv | 3.562 | C36···C15 | 3.5399 |
C14···C48v | 3.4419 | C36···C9i | 3.497 |
C15···C35 | 3.4756 | C37···C14vi | 3.5619 |
C15···C36 | 3.5399 | C39···C21 | 3.5948 |
C16···C13 | 3.2471 | C39···C22 | 3.492 |
C21···C39 | 3.5948 | C39···C23 | 3.5752 |
C22···C26 | 3.2378 | C40···C22 | 3.2019 |
C22···C27 | 3.2656 | C40···C23 | 3.1935 |
C22···C39 | 3.492 | C40···C24 | 3.4508 |
C22···C40 | 3.2019 | C40···C47 | 3.2762 |
C23···C27 | 3.2668 | C43···C2i | 3.4264 |
C23···C35 | 3.3446 | C43···C33i | 3.5483 |
C23···C39 | 3.5752 | C43···C43i | 3.5454 |
C23···C40 | 3.1935 | C47···C33 | 3.246 |
C24···C6 | 3.5828 | C47···C40 | 3.2762 |
C24···C35 | 3.1103 | C48···C3vii | 3.4177 |
C24···C40 | 3.4508 | C48···C14viii | 3.4419 |
| | | |
P1—Pd1—P2 | 90.85 | C15—C24—C23 | 119.27 |
P1—Pd1—P1i | 122.79 | C15—C24—C25 | 122.04 |
P1—Pd1—P2i | 117.49 | C23—C24—C25 | 118.62 |
P1i—Pd1—P2 | 117.49 | C24—C25—C26 | 118.22 |
P2—Pd1—P2i | 120.33 | C24—C25—C34 | 120.72 |
P1i—Pd1—P2i | 90.85 | C26—C25—C34 | 121.05 |
Pd1—P1—C1 | 115.41 | C25—C26—C27 | 123.55 |
Pd1—P1—C8 | 122.62 | C25—C26—C31 | 119.57 |
Pd1—P1—C15 | 111.31 | C27—C26—C31 | 116.83 |
C1—P1—C8 | 100.53 | C26—C27—C28 | 121.67 |
C1—P1—C15 | 105.96 | C27—C28—C29 | 120.75 |
C8—P1—C15 | 98.68 | C28—C29—C30 | 119.47 |
Pd1—P2—C34 | 111.13 | C29—C30—C31 | 121.48 |
Pd1—P2—C35 | 116.89 | C26—C31—C30 | 119.78 |
Pd1—P2—C42 | 121.68 | C26—C31—C32 | 118.22 |
C34—P2—C35 | 104.37 | C30—C31—C32 | 122 |
C34—P2—C42 | 99.68 | C31—C32—C33 | 120.58 |
C35—P2—C42 | 100.53 | C32—C33—C34 | 122.38 |
P1—C1—C2 | 117.38 | P2—C34—C25 | 124.57 |
P1—C1—C6 | 125.16 | P2—C34—C33 | 117.11 |
C2—C1—C6 | 117.45 | C25—C34—C33 | 118.08 |
C1—C2—C3 | 121.79 | P2—C35—C36 | 117.31 |
C2—C3—C4 | 121.43 | P2—C35—C40 | 125.56 |
C3—C4—C5 | 117.55 | C36—C35—C40 | 117.09 |
C3—C4—C7 | 121.32 | C35—C36—C37 | 122.16 |
C5—C4—C7 | 121.13 | C36—C37—C38 | 120.07 |
C4—C5—C6 | 121.56 | C37—C38—C39 | 119.4 |
C1—C6—C5 | 120.21 | C37—C38—C41 | 120.21 |
P1—C8—C9 | 119.87 | C39—C38—C41 | 120.37 |
P1—C8—C13 | 122.44 | C38—C39—C40 | 120.49 |
C9—C8—C13 | 117.69 | C35—C40—C39 | 120.69 |
C8—C9—C10 | 120.49 | P2—C42—C43 | 118.07 |
C9—C10—C11 | 120.74 | P2—C42—C47 | 126.31 |
C10—C11—C12 | 118.22 | C43—C42—C47 | 115.15 |
C10—C11—C14 | 122.14 | C42—C43—C44 | 121.06 |
C12—C11—C14 | 119.63 | C43—C44—C45 | 121.63 |
C11—C12—C13 | 121.56 | C44—C45—C46 | 117.15 |
C8—C13—C12 | 121.3 | C44—C45—C48 | 121.93 |
P1—C15—C16 | 116.78 | C46—C45—C48 | 120.89 |
P1—C15—C24 | 123.52 | C45—C46—C47 | 121.94 |
C16—C15—C24 | 119.55 | C42—C47—C46 | 122.88 |
C15—C16—C17 | 121.25 | C98—C97—C102 | 121.85 |
C16—C17—C18 | 121.52 | C97—C98—C99 | 117.72 |
C17—C18—C19 | 122.44 | C98—C99—C100 | 126.23 |
C17—C18—C23 | 117.35 | C99—C100—C101 | 120.79 |
C19—C18—C23 | 120.2 | C100—C101—C102 | 112.96 |
C18—C19—C20 | 121.67 | C97—C102—C101 | 120.21 |
C19—C20—C21 | 118.39 | C104—C103—C108 | 124.43 |
C20—C21—C22 | 120.63 | C103—C104—C105 | 122.37 |
C21—C22—C23 | 122.62 | C104—C105—C106 | 121.5 |
C18—C23—C22 | 116.46 | C105—C106—C107 | 111.62 |
C18—C23—C24 | 120.98 | C106—C107—C108 | 122.77 |
C22—C23—C24 | 122.56 | C103—C108—C107 | 116.62 |
| | | |
P2—Pd1—P1—C1 | 83.08 | P1—C15—C16—C17 | 172.1 |
P1i—Pd1—P1—C1 | −152.96 | C24—C15—C16—C17 | −3.56 |
P2i—Pd1—P1—C1 | −42.16 | C16—C15—C24—C25 | 178.91 |
P2—Pd1—P1—C8 | −153.95 | P1—C15—C24—C23 | −173.33 |
P1i—Pd1—P1—C8 | −29.99 | C15—C16—C17—C18 | 2.72 |
P2i—Pd1—P1—C8 | 80.81 | C16—C17—C18—C23 | −0.36 |
P2—Pd1—P1—C15 | −37.73 | C16—C17—C18—C19 | −179.21 |
P1i—Pd1—P1—C15 | 86.24 | C23—C18—C19—C20 | 1.34 |
P2i—Pd1—P1—C15 | −162.97 | C19—C18—C23—C24 | 177.74 |
P1—Pd1—P2—C34 | −37.97 | C19—C18—C23—C22 | −1.62 |
P1i—Pd1—P2—C34 | −166.16 | C17—C18—C23—C22 | 179.5 |
P2i—Pd1—P2—C34 | 84.95 | C17—C18—C19—C20 | −179.84 |
P1—Pd1—P2—C35 | 81.65 | C17—C18—C23—C24 | −1.14 |
P1i—Pd1—P2—C35 | −46.54 | C18—C19—C20—C21 | 0.28 |
P2i—Pd1—P2—C35 | −155.43 | C19—C20—C21—C22 | −1.56 |
P1—Pd1—P2—C42 | −154.73 | C20—C21—C22—C23 | 1.25 |
P1i—Pd1—P2—C42 | 77.08 | C21—C22—C23—C24 | −178.99 |
P2i—Pd1—P2—C42 | −31.81 | C21—C22—C23—C18 | 0.36 |
Pd1—P1—C1—C2 | 19.61 | C18—C23—C24—C25 | −176.70 |
C8—P1—C1—C2 | −114.43 | C18—C23—C24—C15 | 0.29 |
C15—P1—C1—C2 | 143.28 | C22—C23—C24—C25 | 2.62 |
Pd1—P1—C1—C6 | −161.54 | C22—C23—C24—C15 | 179.62 |
C8—P1—C1—C6 | 64.41 | C23—C24—C25—C26 | −71.98 |
C15—P1—C1—C6 | −37.87 | C15—C24—C25—C34 | −69.83 |
C8—P1—C15—C24 | −152.93 | C15—C24—C25—C26 | 111.12 |
C15—P1—C8—C13 | 59.33 | C23—C24—C25—C34 | 107.08 |
C1—P1—C15—C24 | −49.29 | C24—C25—C34—P2 | 4.55 |
Pd1—P1—C8—C9 | 0.84 | C26—C25—C34—P2 | −176.42 |
C1—P1—C8—C9 | 130.41 | C26—C25—C34—C33 | −2.25 |
C15—P1—C8—C9 | −121.45 | C24—C25—C26—C27 | −0.30 |
Pd1—P1—C8—C13 | −178.38 | C24—C25—C26—C31 | −177.70 |
C1—P1—C8—C13 | −48.81 | C24—C25—C34—C33 | 178.73 |
Pd1—P1—C15—C24 | 76.91 | C34—C25—C26—C31 | 3.25 |
Pd1—P1—C15—C16 | −98.56 | C34—C25—C26—C27 | −179.35 |
C1—P1—C15—C16 | 135.24 | C27—C26—C31—C32 | −178.69 |
C8—P1—C15—C16 | 31.6 | C25—C26—C27—C28 | −179.27 |
C35—P2—C42—C47 | −52.13 | C31—C26—C27—C28 | −1.80 |
C34—P2—C35—C40 | −44.42 | C25—C26—C31—C30 | 179.22 |
C35—P2—C34—C33 | 134.82 | C25—C26—C31—C32 | −1.11 |
C42—P2—C35—C40 | 58.53 | C27—C26—C31—C30 | 1.65 |
Pd1—P2—C34—C33 | −98.34 | C26—C27—C28—C29 | 0.93 |
Pd1—P2—C35—C40 | −167.59 | C27—C28—C29—C30 | 0.16 |
Pd1—P2—C42—C47 | 176.93 | C28—C29—C30—C31 | −0.29 |
C42—P2—C35—C36 | −123.89 | C29—C30—C31—C32 | 179.7 |
Pd1—P2—C34—C25 | 75.89 | C29—C30—C31—C26 | −0.65 |
C35—P2—C34—C25 | −50.95 | C30—C31—C32—C33 | 177.66 |
C42—P2—C34—C25 | −154.54 | C26—C31—C32—C33 | −2.00 |
C34—P2—C42—C47 | 54.59 | C31—C32—C33—C34 | 3.1 |
C35—P2—C42—C43 | 136.13 | C32—C33—C34—P2 | 173.65 |
C34—P2—C35—C36 | 133.15 | C32—C33—C34—C25 | −0.96 |
Pd1—P2—C42—C43 | 5.19 | P2—C35—C40—C39 | −179.03 |
C34—P2—C42—C43 | −117.15 | C40—C35—C36—C37 | −1.56 |
Pd1—P2—C35—C36 | 9.98 | P2—C35—C36—C37 | −179.34 |
C42—P2—C34—C33 | 31.23 | C36—C35—C40—C39 | 3.4 |
P1—C1—C2—C3 | 178.15 | C35—C36—C37—C38 | −1.08 |
P1—C1—C6—C5 | −177.79 | C36—C37—C38—C39 | 1.85 |
C6—C1—C2—C3 | −0.78 | C36—C37—C38—C41 | −179.74 |
C2—C1—C6—C5 | 1.06 | C41—C38—C39—C40 | −178.41 |
C1—C2—C3—C4 | −0.08 | C37—C38—C39—C40 | 0 |
C2—C3—C4—C5 | 0.66 | C38—C39—C40—C35 | −2.71 |
C2—C3—C4—C7 | −178.62 | P2—C42—C43—C44 | 174.29 |
C3—C4—C5—C6 | −0.36 | C47—C42—C43—C44 | 1.64 |
C7—C4—C5—C6 | 178.91 | P2—C42—C47—C46 | −175.69 |
C4—C5—C6—C1 | −0.51 | C43—C42—C47—C46 | −3.75 |
P1—C8—C9—C10 | −179.52 | C42—C43—C44—C45 | −0.96 |
P1—C8—C13—C12 | 179.86 | C43—C44—C45—C46 | 2.16 |
C13—C8—C9—C10 | −0.26 | C43—C44—C45—C48 | −176.09 |
C9—C8—C13—C12 | 0.62 | C44—C45—C46—C47 | −4.24 |
C8—C9—C10—C11 | −0.19 | C48—C45—C46—C47 | 174.03 |
C9—C10—C11—C12 | 0.29 | C45—C46—C47—C42 | 5.3 |
C9—C10—C11—C14 | 178.56 | C102—C97—C98—C99 | 2.27 |
C14—C11—C12—C13 | −178.24 | C98—C97—C102—C101 | 1.34 |
C10—C11—C12—C13 | 0.07 | C97—C98—C99—C100 | −5.86 |
C11—C12—C13—C8 | −0.54 | C98—C99—C100—C101 | 5.51 |
C16—C15—C24—C23 | 2.02 | C99—C100—C101—C102 | −1.38 |
P1—C15—C24—C25 | 3.56 | | |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, −y+1, z+1/2; (iii) x, −y, −z+1; (iv) −x, −y, z+1/2; (v) −x, y−1, −z+1/2; (vi) −x, −y, z−1/2; (vii) −x, −y+1, z−1/2; (viii) −x, y+1, −z+1/2. |
(15) bis(4-Amin-
N-2-thiazolylbenzenesulfonamide-
N)-dichloro-methanl-copper(ii) bis(Sulfathiazole-
N)-dichloro-methanl-copper(ii)
top
Crystal data top
C19H22Cl2CuN6O5S4 | γ = 90° |
Mr = 677.16 | V = 2516 (3) Å3 |
Monclinic, I2/a | Z = 4 |
Hall symbol: -I 2ya | F(000) = 1292 |
a = 30.123 (13) Å | Dx = 1.729 Mg m−3 |
b = 7.564 (6) Å | Mo Kα radiation, λ = 0.71073 Å |
c = 11.044 (6) Å | µ = 1.46 mm−1 |
α = 90° | T = 293 K |
β = 91.27 (1)° | × × mm |
Data collection top
Radiation source: fine-focus sealed tube | θmax = 27.6°, θmin = 3.4° |
3814 measured reflections | h = −12→35 |
2078 independent reflections | k = −8→9 |
2062 reflections with I > 2σ(I) | l = −12→13 |
Rint = 0.069 | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.053 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.156 | w = 1/[σ2(Fo2) + (0.0576P)2 + 14.5807P] where P = (Fo2 + 2Fc2)/3 |
S = 1.16 | (Δ/σ)max < 0.001 |
2078 reflections | Δρmax = 0.70 e Å−3 |
173 parameters | Δρmin = −0.90 e Å−3 |
0 restraints | Extinction correction: nne |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
C19H22Cl2CuN6O5S4 | γ = 90° |
Mr = 677.16 | V = 2516 (3) Å3 |
Monclinic, I2/a | Z = 4 |
a = 30.123 (13) Å | Mo Kα radiation |
b = 7.564 (6) Å | µ = 1.46 mm−1 |
c = 11.044 (6) Å | T = 293 K |
α = 90° | × × mm |
β = 91.27 (1)° | |
Data collection top
3814 measured reflections | 2062 reflections with I > 2σ(I) |
2078 independent reflections | Rint = 0.069 |
Refinement top
R[F2 > 2σ(F2)] = 0.053 | 0 restraints |
wR(F2) = 0.156 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0576P)2 + 14.5807P] where P = (Fo2 + 2Fc2)/3 |
2078 reflections | Δρmax = 0.70 e Å−3 |
173 parameters | Δρmin = −0.90 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is nt relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cu1 | 0.2500 | 0.34015 (10) | 0.5000 | 0.0295 (3) | |
Cl1 | 0.28148 (4) | 0.4227 (2) | 0.32840 (11) | 0.0518 (4) | |
S1 | 0.09795 (4) | 0.99494 (16) | 0.38474 (11) | 0.0351 (3) | |
S2 | 0.02339 (5) | 0.9338 (2) | 0.17310 (12) | 0.0518 (4) | |
O1 | 0.10452 (12) | 1.0688 (5) | 0.2698 (4) | 0.0517 (10) | |
O2 | 0.11481 (12) | 1.0872 (5) | 0.4873 (4) | 0.0492 (10) | |
O5 | 0.2468 (3) | 0.0425 (10) | 0.5545 (7) | 0.0507 (19) | 0.50 |
N1 | 0.19059 (12) | 0.3159 (5) | 0.4140 (4) | 0.0332 (9) | |
N2 | 0.04656 (12) | 0.9685 (6) | 0.4120 (3) | 0.0338 (9) | |
N3 | −0.02552 (13) | 0.9384 (6) | 0.3512 (4) | 0.0369 (9) | |
C1 | 0.16547 (14) | 0.4738 (6) | 0.4012 (4) | 0.0294 (9) | |
C2 | 0.13727 (14) | 0.5210 (7) | 0.4913 (4) | 0.0314 (10) | |
C3 | 0.11592 (14) | 0.6786 (7) | 0.4835 (4) | 0.0322 (10) | |
C4 | 0.12186 (13) | 0.7872 (6) | 0.3866 (4) | 0.0294 (9) | |
C5 | 0.14925 (15) | 0.7384 (7) | 0.2949 (4) | 0.0359 (11) | |
C6 | 0.17105 (16) | 0.5807 (7) | 0.3031 (4) | 0.0372 (11) | |
C7 | 0.01734 (15) | 0.9490 (6) | 0.3255 (4) | 0.0317 (10) | |
C8 | −0.05359 (18) | 0.9180 (8) | 0.2530 (5) | 0.0457 (13) | |
C9 | −0.0326 (2) | 0.9106 (9) | 0.1505 (5) | 0.0529 (14) | |
C19 | 0.2500 | −0.1134 (13) | 0.5000 | 0.079 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0270 (4) | 0.0269 (4) | 0.0350 (5) | 0.000 | 0.0088 (3) | 0.000 |
Cl1 | 0.0417 (7) | 0.0806 (11) | 0.0333 (6) | −0.0263 (7) | 0.0097 (5) | −0.0086 (7) |
S1 | 0.0252 (6) | 0.0342 (7) | 0.0463 (7) | −0.0003 (4) | 0.0104 (5) | 0.0050 (5) |
S2 | 0.0508 (8) | 0.0694 (10) | 0.0354 (7) | 0.0055 (7) | 0.0079 (6) | −0.0017 (7) |
O1 | 0.042 (2) | 0.052 (2) | 0.062 (2) | 0.0108 (17) | 0.0236 (18) | 0.024 (2) |
O2 | 0.039 (2) | 0.040 (2) | 0.069 (3) | −0.0082 (16) | 0.0035 (17) | −0.012 (2) |
O5 | 0.073 (5) | 0.035 (4) | 0.043 (4) | −0.010 (4) | −0.009 (4) | 0.004 (3) |
N1 | 0.0285 (19) | 0.0277 (19) | 0.044 (2) | 0.0000 (15) | 0.0053 (16) | −0.0025 (17) |
N2 | 0.0208 (18) | 0.044 (2) | 0.036 (2) | 0.0033 (16) | 0.0063 (15) | 0.0026 (19) |
N3 | 0.0254 (19) | 0.041 (2) | 0.045 (2) | 0.0028 (17) | 0.0013 (16) | −0.003 (2) |
C1 | 0.026 (2) | 0.031 (2) | 0.032 (2) | −0.0031 (17) | 0.0026 (17) | −0.005 (2) |
C2 | 0.025 (2) | 0.039 (3) | 0.031 (2) | −0.0004 (18) | 0.0044 (17) | 0.003 (2) |
C3 | 0.025 (2) | 0.042 (3) | 0.030 (2) | −0.0014 (19) | 0.0063 (17) | 0.001 (2) |
C4 | 0.021 (2) | 0.033 (2) | 0.034 (2) | −0.0026 (17) | 0.0044 (17) | 0.000 (2) |
C5 | 0.031 (2) | 0.043 (3) | 0.034 (2) | −0.001 (2) | 0.0088 (18) | 0.004 (2) |
C6 | 0.037 (3) | 0.043 (3) | 0.033 (2) | 0.001 (2) | 0.0120 (19) | 0.000 (2) |
C7 | 0.030 (2) | 0.029 (2) | 0.036 (2) | 0.0046 (18) | 0.0063 (19) | 0.003 (2) |
C8 | 0.039 (3) | 0.044 (3) | 0.053 (3) | 0.004 (2) | −0.010 (2) | −0.006 (3) |
C9 | 0.053 (3) | 0.056 (4) | 0.049 (3) | 0.004 (3) | −0.007 (3) | −0.005 (3) |
C19 | 0.116 (9) | 0.036 (5) | 0.084 (8) | 0.000 | −0.006 (6) | 0.000 |
Geometric parameters (Å, º) top
Cu1—N1i | 2.016 (4) | O5—C19 | 1.329 (12) |
Cu1—N1 | 2.016 (4) | N1—C1 | 1.419 (6) |
Cu1—Cl1i | 2.2270 (15) | N2—C7 | 1.293 (6) |
Cu1—Cl1 | 2.2270 (15) | N3—C7 | 1.330 (6) |
Cu1—O5i | 2.333 (8) | N3—C8 | 1.368 (7) |
Cu1—O5 | 2.333 (8) | C1—C6 | 1.365 (7) |
S1—O1 | 1.404 (4) | C1—C2 | 1.370 (6) |
S1—O2 | 1.415 (4) | C2—C3 | 1.356 (7) |
S1—N2 | 1.596 (4) | C3—C4 | 1.365 (6) |
S1—C4 | 1.729 (5) | C4—C5 | 1.371 (6) |
S2—C7 | 1.701 (5) | C5—C6 | 1.364 (7) |
S2—C9 | 1.710 (6) | C8—C9 | 1.310 (9) |
O5—O5i | 1.223 (15) | C19—O5i | 1.329 (12) |
| | | |
N1i—Cu1—N1 | 169.6 (2) | O5i—O5—C19 | 62.6 (4) |
N1i—Cu1—Cl1i | 90.85 (12) | O5i—O5—Cu1 | 74.81 (19) |
N1—Cu1—Cl1i | 92.07 (12) | C19—O5—Cu1 | 137.4 (5) |
N1i—Cu1—Cl1 | 92.07 (12) | C1—N1—Cu1 | 115.9 (3) |
N1—Cu1—Cl1 | 90.85 (12) | C7—N2—S1 | 121.5 (3) |
Cl1i—Cu1—Cl1 | 147.45 (10) | C7—N3—C8 | 115.1 (4) |
N1i—Cu1—O5i | 89.5 (2) | C6—C1—C2 | 120.7 (4) |
N1—Cu1—O5i | 80.4 (2) | C6—C1—N1 | 120.2 (4) |
Cl1i—Cu1—O5i | 120.7 (2) | C2—C1—N1 | 119.0 (4) |
Cl1—Cu1—O5i | 91.7 (2) | C3—C2—C1 | 118.9 (4) |
N1i—Cu1—O5 | 80.4 (2) | C2—C3—C4 | 120.6 (4) |
N1—Cu1—O5 | 89.5 (2) | C3—C4—C5 | 120.6 (4) |
Cl1i—Cu1—O5 | 91.7 (2) | C3—C4—S1 | 119.6 (3) |
Cl1—Cu1—O5 | 120.7 (2) | C5—C4—S1 | 119.6 (4) |
O5i—Cu1—O5 | 30.4 (4) | C6—C5—C4 | 118.9 (5) |
O1—S1—O2 | 118.2 (3) | C5—C6—C1 | 120.2 (4) |
O1—S1—N2 | 112.1 (2) | N2—C7—N3 | 119.9 (4) |
O2—S1—N2 | 104.1 (2) | N2—C7—S2 | 130.7 (4) |
O1—S1—C4 | 107.8 (2) | N3—C7—S2 | 109.4 (4) |
O2—S1—C4 | 107.3 (2) | C9—C8—N3 | 112.9 (5) |
N2—S1—C4 | 106.8 (2) | C8—C9—S2 | 111.2 (4) |
C7—S2—C9 | 91.4 (3) | O5i—C19—O5 | 54.8 (8) |
| | | |
N1i—Cu1—O5—O5i | −105.9 (8) | C2—C3—C4—S1 | −174.6 (4) |
N1—Cu1—O5—O5i | 71.5 (8) | O1—S1—C4—C3 | −172.8 (4) |
Cl1i—Cu1—O5—O5i | 163.6 (8) | O2—S1—C4—C3 | 59.0 (4) |
Cl1—Cu1—O5—O5i | −19.2 (9) | N2—S1—C4—C3 | −52.1 (4) |
N1i—Cu1—O5—C19 | −105.9 (8) | O1—S1—C4—C5 | 12.0 (5) |
N1—Cu1—O5—C19 | 71.5 (8) | O2—S1—C4—C5 | −116.2 (4) |
Cl1i—Cu1—O5—C19 | 163.6 (8) | N2—S1—C4—C5 | 132.7 (4) |
Cl1—Cu1—O5—C19 | −19.2 (9) | C3—C4—C5—C6 | −1.1 (7) |
O5i—Cu1—O5—C19 | 0.000 (2) | S1—C4—C5—C6 | 174.1 (4) |
N1i—Cu1—N1—C1 | 169.6 (3) | C4—C5—C6—C1 | 0.1 (8) |
Cl1i—Cu1—N1—C1 | 63.4 (3) | C2—C1—C6—C5 | 1.4 (7) |
Cl1—Cu1—N1—C1 | −84.2 (3) | N1—C1—C6—C5 | −175.4 (4) |
O5i—Cu1—N1—C1 | −175.8 (4) | S1—N2—C7—N3 | −175.8 (4) |
O5—Cu1—N1—C1 | 155.1 (4) | S1—N2—C7—S2 | 3.9 (7) |
O1—S1—N2—C7 | 25.7 (5) | C8—N3—C7—N2 | 180.0 (5) |
O2—S1—N2—C7 | 154.6 (4) | C8—N3—C7—S2 | 0.2 (6) |
C4—S1—N2—C7 | −92.1 (4) | C9—S2—C7—N2 | 179.5 (5) |
Cu1—N1—C1—C6 | 88.3 (5) | C9—S2—C7—N3 | −0.8 (4) |
Cu1—N1—C1—C2 | −88.6 (4) | C7—N3—C8—C9 | 0.7 (7) |
C6—C1—C2—C3 | −1.9 (7) | N3—C8—C9—S2 | −1.3 (7) |
N1—C1—C2—C3 | 174.9 (4) | C7—S2—C9—C8 | 1.2 (5) |
C1—C2—C3—C4 | 1.0 (7) | Cu1—O5—C19—O5i | 0.000 (2) |
C2—C3—C4—C5 | 0.5 (7) | | |
Symmetry code: (i) −x+1/2, y, −z+1. |
(16)
catena-(tetrakis(mu!2$-4-Aminbenzoato)-diaqua-di-cadmium tetrahydrate)
top
Crystal data top
C14H14CdN2O5·2(H2O) | γ = 90° |
Mr = 438.71 | V = 1623.2 (3) Å3 |
Monclinic, C2/c | Z = 4 |
Hall symbol: -C 2yc | F(000) = 808 |
a = 15.2963 (19) Å | Dx = 1.721 Mg m−3 |
b = 6.2028 (7) Å | Mo K\a radiation, λ = 0.71073 Å |
c = 17.8150 (18) Å | µ = 1.38 mm−1 |
α = 90° | T = 0 K |
β = 106.196 (4)° | × × mm |
Crystal data top
C14H14CdN2O5·2(H2O) | γ = 90° |
Mr = 438.71 | V = 1623.2 (3) Å3 |
Monclinic, C2/c | Z = 4 |
a = 15.2963 (19) Å | Mo K\a radiation |
b = 6.2028 (7) Å | µ = 1.38 mm−1 |
c = 17.8150 (18) Å | T = 0 K |
α = 90° | × × mm |
β = 106.196 (4)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0 | −0.17340 | 0.25 | 0.02* | |
O1 | 0.08205 | −0.22035 | 0.158 | 0.02* | |
O2 | 0.0499 | 0.1135 | 0.17995 | 0.02* | |
O5 | 0 | −0.54260 | 0.25 | 0.02* | |
N1 | 0.1433 | 0.20835 | −0.14825 | 0.02* | |
C1 | 0.07967 | −0.02288 | 0.1405 | 0.02* | |
C2 | 0.1073 | 0.04715 | 0.07045 | 0.02* | |
C3 | 0.13842 | −0.10448 | 0.0268 | 0.02* | |
C4 | 0.15397 | −0.05058 | −0.04390 | 0.02* | |
C5 | 0.13778 | 0.15778 | −0.07225 | 0.02* | |
C6 | 0.10932 | 0.31343 | −0.02725 | 0.02* | |
C7 | 0.09412 | 0.25853 | 0.04295 | 0.02* | |
O6 | 0.2574 | 0.06635 | 0.28135 | 0.02* | |
Geometric parameters (Å, º) top
Cd1—O1 | 2.3439 | C1—C2 | 1.4896 |
Cd1—O2 | 2.4162 | C2—C3 | 1.3865 |
Cd1—O5 | 2.2901 (3) | C2—C7 | 1.3945 |
Cd1—C1 | 2.7365 | C3—C4 | 1.3863 |
O1—C1 | 1.2619 | C4—C5 | 1.3845 |
O2—C1 | 1.2631 | C5—C6 | 1.3996 |
N1—C5 | 1.4151 | C6—C7 | 1.377 |
| | | |
Cd1···O5i | 3.9127 (5) | O6···O2 | 3.1976 |
Cd1···O6 | 4.0986 | O6···C1 | 3.1919 |
Cd1···O5ii | 3.9127 (5) | O6···Cd1 | 4.0986 |
Cd1···O6iii | 4.0986 | O6···Cd1 | 4.0986 |
O1···C6iv | 3.2441 | N1···O6x | 2.9569 |
O1···O6v | 2.7329 | C1···C6iv | 3.5245 |
O2···O5i | 2.6873 | C1···C4iv | 3.537 |
O2···O6 | 3.1976 | C1···O6 | 3.1919 |
O2···O5ii | 2.6873 | C2···C2iv | 3.5807 |
O2···C4iv | 3.3963 | C3···C7iv | 3.5558 |
O5···Cd1vi | 3.9127 (5) | C4···O2iv | 3.3963 |
O5···O2vi | 2.6873 | C4···C1iv | 3.537 |
O5···Cd1vii | 3.9127 (5) | C6···C1iv | 3.5245 |
O5···O2vii | 2.6873 | C6···O1iv | 3.2441 |
O6···N1viii | 2.9569 | C7···C3iv | 3.5558 |
O6···O1ix | 2.7329 | | |
| | | |
O1—Cd1—O2 | 54.72 | O1iii—Cd1—N1iv | 87.88 |
O1—Cd1—O5 | 82.86 | O1iii—Cd1—N1viii | 90.85 |
O1—Cd1—C1 | 27.39 | O2iii—Cd1—C1iii | 27.49 |
O1—Cd1—O1iii | 165.73 | O2iii—Cd1—N1iv | 95.84 |
O1—Cd1—O2iii | 139.51 | O2iii—Cd1—N1viii | 91.69 |
O1—Cd1—C1iii | 166.57 | N1iv—Cd1—C1iii | 94.23 |
O1—Cd1—N1iv | 90.85 | N1viii—Cd1—C1iii | 89.26 |
O1—Cd1—N1viii | 87.88 | N1iv—Cd1—N1viii | 169.78 |
O2—Cd1—O5 | 137.43 | Cd1—O1—C1 | 93.9 |
O2—Cd1—C1 | 27.49 | Cd1—O2—C1 | 90.51 |
O1iii—Cd1—O2 | 139.51 | Cd1iv—N1—C5 | 114.28 |
O2—Cd1—O2iii | 85.13 | Cd1—C1—O1 | 58.71 |
O2—Cd1—C1iii | 112.62 | Cd1—C1—O2 | 62 |
O2—Cd1—N1iv | 91.69 | Cd1—C1—C2 | 169.59 |
O2—Cd1—N1viii | 95.84 | O1—C1—O2 | 120.17 |
O5—Cd1—C1 | 109.95 | O1—C1—C2 | 119.65 |
O1iii—Cd1—O5 | 82.86 | O2—C1—C2 | 120.09 |
O2iii—Cd1—O5 | 137.43 | C1—C2—C3 | 119.61 |
O5—Cd1—C1iii | 109.95 | C1—C2—C7 | 121.43 |
O5—Cd1—N1iv | 84.89 | C3—C2—C7 | 118.64 |
O5—Cd1—N1viii | 84.89 | C2—C3—C4 | 121.25 |
O1iii—Cd1—C1 | 166.57 | C3—C4—C5 | 119.87 |
O2iii—Cd1—C1 | 112.62 | N1—C5—C4 | 120.24 |
C1—Cd1—C1iii | 140.1 | N1—C5—C6 | 120.41 |
N1iv—Cd1—C1 | 89.26 | C4—C5—C6 | 119.18 |
N1viii—Cd1—C1 | 94.23 | C5—C6—C7 | 120.52 |
O1iii—Cd1—O2iii | 54.72 | C2—C7—C6 | 120.47 |
O1iii—Cd1—C1iii | 27.39 | | |
| | | |
O2—Cd1—O1—C1 | −4.72 | N1iv—Cd1—C1—O2 | 95.1 |
O5—Cd1—O1—C1 | 171.5 | N1viii—Cd1—C1—O2 | −94.52 |
O2iii—Cd1—O1—C1 | −13.26 | Cd1—O1—C1—O2 | 8.55 |
N1iv—Cd1—O1—C1 | 86.75 | Cd1—O1—C1—C2 | −168.07 |
N1viii—Cd1—O1—C1 | −103.39 | Cd1—O2—C1—O1 | −8.27 |
O1—Cd1—O2—C1 | 4.71 | Cd1—O2—C1—C2 | 168.33 |
O5—Cd1—O2—C1 | −0.85 | Cd1iv—N1—C5—C4 | 91 |
O1iii—Cd1—O2—C1 | −173.86 | Cd1iv—N1—C5—C6 | −84.19 |
O2iii—Cd1—O2—C1 | 179.15 | O1—C1—C2—C3 | −2.28 |
C1iii—Cd1—O2—C1 | 179.58 | O2—C1—C2—C7 | −5.43 |
N1iv—Cd1—O2—C1 | −85.13 | O1—C1—C2—C7 | 171.19 |
N1viii—Cd1—O2—C1 | 87.94 | O2—C1—C2—C3 | −178.90 |
O2—Cd1—C1—O1 | 171.63 | C1—C2—C7—C6 | −171.72 |
O5—Cd1—C1—O1 | −8.98 | C3—C2—C7—C6 | 1.82 |
O2iii—Cd1—C1—O1 | 170.71 | C1—C2—C3—C4 | 171.88 |
C1iii—Cd1—C1—O1 | 171.02 | C7—C2—C3—C4 | −1.77 |
N1iv—Cd1—C1—O1 | −93.27 | C2—C3—C4—C5 | −0.43 |
N1viii—Cd1—C1—O1 | 77.11 | C3—C4—C5—C6 | 2.57 |
O1—Cd1—C1—O2 | −171.63 | C3—C4—C5—N1 | −172.69 |
O5—Cd1—C1—O2 | 179.39 | N1—C5—C6—C7 | 172.72 |
O2iii—Cd1—C1—O2 | −0.92 | C4—C5—C6—C7 | −2.53 |
C1iii—Cd1—C1—O2 | −0.61 | C5—C6—C7—C2 | 0.32 |
Symmetry codes: (i) x, y+1, z; (ii) −x, y+1, −z+1/2; (iii) −x, y, −z+1/2; (iv) −x, −y, −z; (v) −x+1/2, y−1/2, −z+1/2; (vi) x, y−1, z; (vii) −x, y−1, −z+1/2; (viii) x, −y, z+1/2; (ix) −x+1/2, y+1/2, −z+1/2; (x) x, −y, z−1/2. |
(17) 4-Ferrocenylmethylene-2-phenyl-4
H-oxazol-5-one
top
Crystal data top
C20H15FeNO2 | γ = 90° |
Mr = 357.18 | V = 1543.8 (7) Å3 |
Monclinic, P21/n | Z = 4 |
Hall symbol: -P 2yn | F(000) = 676 |
a = 10.391 (2) Å | Dx = 1.472 Mg m−3 |
b = 7.252 (3) Å | Mo K\a radiation, λ = 0.71070 Å |
c = 20.662 (2) Å | µ = 0.99 mm−1 |
α = 90° | T = 0 K |
β = 97.47 (2)° | × × mm |
Crystal data top
C20H15FeNO2 | γ = 90° |
Mr = 357.18 | V = 1543.8 (7) Å3 |
Monclinic, P21/n | Z = 4 |
a = 10.391 (2) Å | Mo K\a radiation |
b = 7.252 (3) Å | µ = 0.99 mm−1 |
c = 20.662 (2) Å | T = 0 K |
α = 90° | × × mm |
β = 97.47 (2)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe1 | 0.49402 | 0.28301 | 0.22699 | 0.02* | |
O1 | 0.34705 | 0.28975 | −0.05861 | 0.02* | |
O2 | 0.1385 | 0.24945 | −0.04154 | 0.02* | |
N1 | 0.1493 | 0.31655 | 0.06581 | 0.02* | |
C1 | 0.3939 | 0.43825 | 0.15402 | 0.02* | |
C2 | 0.31085 | 0.3841 | 0.20045 | 0.02* | |
C3 | 0.36435 | 0.4541 | 0.2621 | 0.02* | |
C4 | 0.47905 | 0.54870 | 0.25466 | 0.02* | |
C5 | 0.4999 | 0.539 | 0.18883 | 0.02* | |
C6 | 0.48825 | 0.0034 | 0.23119 | 0.02* | |
C7 | 0.52585 | 0.07665 | 0.29383 | 0.02* | |
C8 | 0.64060 | 0.17875 | 0.29176 | 0.02* | |
C9 | 0.6727 | 0.16850 | 0.22756 | 0.02* | |
C10 | 0.579 | 0.05885 | 0.19063 | 0.02* | |
C11 | 0.3817 | 0.39485 | 0.08556 | 0.02* | |
C12 | 0.2734 | 0.3376 | 0.04803 | 0.02* | |
C13 | 0.2681 | 0.29385 | −0.02152 | 0.02* | |
C14 | 0.07625 | 0.2689 | 0.01369 | 0.02* | |
C15 | −0.06255 | 0.23475 | 0.00547 | 0.02* | |
C16 | −0.13250 | 0.2691 | 0.05718 | 0.02* | |
C17 | −0.26390 | 0.2399 | 0.05005 | 0.02* | |
C18 | −0.32790 | 0.1749 | −0.00840 | 0.02* | |
C19 | −0.25940 | 0.14025 | −0.05944 | 0.02* | |
C20 | −0.12735 | 0.1705 | −0.05305 | 0.02* | |
Geometric parameters (Å, º) top
Fe1—C1 | 2.0531 | C2—C3 | 1.4161 |
Fe1—C2 | 2.0468 | C3—C4 | 1.4009 |
Fe1—C3 | 2.0336 | C4—C5 | 1.4066 |
Fe1—C4 | 2.0216 | C6—C7 | 1.4066 |
Fe1—C5 | 2.0210 | C6—C10 | 1.3995 |
Fe1—C6 | 2.0308 | C7—C8 | 1.4089 |
Fe1—C7 | 2.0341 | C8—C9 | 1.4112 |
Fe1—C8 | 2.0378 | C9—C10 | 1.4033 |
Fe1—C9 | 2.0326 | C11—C12 | 1.3465 |
Fe1—C10 | 2.0394 | C12—C13 | 1.4657 |
O1—C13 | 1.1936 | C14—C15 | 1.4514 |
O2—C13 | 1.3941 | C15—C16 | 1.3906 |
O2—C14 | 1.3901 | C15—C20 | 1.3859 |
N1—C12 | 1.3944 | C16—C17 | 1.3706 |
N1—C14 | 1.2817 | C17—C18 | 1.3835 |
C1—C2 | 1.4264 | C18—C19 | 1.3701 |
C1—C5 | 1.4347 | C19—C20 | 1.3788 |
C1—C11 | 1.4385 | | |
| | | |
N1···C2 | 3.0956 | C13···C19iv | 3.5716 |
C2···N1 | 3.0956 | C14···C19iv | 3.5849 |
C4···C6i | 3.3361 | C14···C20iv | 3.3144 |
C5···C6i | 3.4858 | C16···C13iii | 3.5077 |
C6···C4ii | 3.3361 | C17···C13iii | 3.4315 |
C6···C5ii | 3.4858 | C18···C11iii | 3.5154 |
C11···C18iii | 3.5154 | C18···C13iv | 3.4963 |
C12···C19iv | 3.4777 | C19···C12iv | 3.4777 |
C13···C16iii | 3.5077 | C19···C13iv | 3.5716 |
C13···C17iii | 3.4315 | C19···C14iv | 3.5849 |
C13···C18iv | 3.4963 | C20···C14iv | 3.3144 |
| | | |
C1—Fe1—C2 | 40.72 | Fe1—C1—C11 | 125 |
C1—Fe1—C3 | 68.37 | C2—C1—C5 | 107.17 |
C1—Fe1—C4 | 68.58 | C2—C1—C11 | 128.13 |
C1—Fe1—C5 | 41.23 | C5—C1—C11 | 124.62 |
C1—Fe1—C6 | 124.33 | Fe1—C2—C1 | 69.88 |
C1—Fe1—C7 | 157.54 | Fe1—C2—C3 | 69.19 |
C1—Fe1—C8 | 161.78 | C1—C2—C3 | 107.77 |
C1—Fe1—C9 | 127.13 | Fe1—C3—C2 | 70.2 |
C1—Fe1—C10 | 111.65 | Fe1—C3—C4 | 69.33 |
C2—Fe1—C3 | 40.61 | C2—C3—C4 | 108.48 |
C2—Fe1—C4 | 68.37 | Fe1—C4—C3 | 70.25 |
C2—Fe1—C5 | 68.94 | Fe1—C4—C5 | 69.62 |
C2—Fe1—C6 | 109.72 | C3—C4—C5 | 108.77 |
C2—Fe1—C7 | 120.59 | Fe1—C5—C1 | 70.59 |
C2—Fe1—C8 | 153.96 | Fe1—C5—C4 | 69.66 |
C2—Fe1—C9 | 164.75 | C1—C5—C4 | 107.79 |
C2—Fe1—C10 | 128.23 | Fe1—C6—C7 | 69.88 |
C3—Fe1—C4 | 40.42 | Fe1—C6—C10 | 70.22 |
C3—Fe1—C5 | 68.52 | C7—C6—C10 | 108.32 |
C3—Fe1—C6 | 124.71 | Fe1—C7—C6 | 69.63 |
C3—Fe1—C7 | 105.28 | Fe1—C7—C8 | 69.9 |
C3—Fe1—C8 | 117.74 | C6—C7—C8 | 107.79 |
C3—Fe1—C9 | 153.42 | Fe1—C8—C7 | 69.62 |
C3—Fe1—C10 | 163.03 | Fe1—C8—C9 | 69.52 |
C4—Fe1—C5 | 40.72 | C7—C8—C9 | 107.77 |
C4—Fe1—C6 | 159.36 | Fe1—C9—C8 | 69.91 |
C4—Fe1—C7 | 121.39 | Fe1—C9—C10 | 70.1 |
C4—Fe1—C8 | 104.26 | C8—C9—C10 | 107.99 |
C4—Fe1—C9 | 119.45 | Fe1—C10—C6 | 69.56 |
C4—Fe1—C10 | 156.47 | Fe1—C10—C9 | 69.58 |
C5—Fe1—C6 | 159.46 | C6—C10—C9 | 108.12 |
C5—Fe1—C7 | 158.47 | C1—C11—C12 | 126.44 |
C5—Fe1—C8 | 122.62 | N1—C12—C11 | 127.9 |
C5—Fe1—C9 | 107.68 | N1—C12—C13 | 108.45 |
C5—Fe1—C10 | 123.5 | C11—C12—C13 | 123.6 |
C6—Fe1—C7 | 40.49 | O1—C13—O2 | 121.45 |
C6—Fe1—C8 | 67.99 | O1—C13—C12 | 133.91 |
C6—Fe1—C9 | 67.9 | O2—C13—C12 | 104.63 |
C6—Fe1—C10 | 40.22 | O2—C14—N1 | 115.41 |
C7—Fe1—C8 | 40.49 | O2—C14—C15 | 116.61 |
C7—Fe1—C9 | 68.14 | N1—C14—C15 | 127.97 |
C7—Fe1—C10 | 67.9 | C14—C15—C16 | 119.35 |
C8—Fe1—C9 | 40.57 | C14—C15—C20 | 121.48 |
C8—Fe1—C10 | 67.9 | C16—C15—C20 | 119.17 |
C9—Fe1—C10 | 40.32 | C15—C16—C17 | 120.17 |
C13—O2—C14 | 105.52 | C16—C17—C18 | 120.37 |
C12—N1—C14 | 105.97 | C17—C18—C19 | 119.7 |
Fe1—C1—C2 | 69.4 | C18—C19—C20 | 120.48 |
Fe1—C1—C5 | 68.19 | C15—C20—C19 | 120.1 |
| | | |
C3—Fe1—C1—C2 | −37.70 | C9—Fe1—C6—C7 | 81.76 |
C4—Fe1—C1—C2 | −81.30 | C10—Fe1—C6—C7 | 119.17 |
C5—Fe1—C1—C2 | −119.35 | C8—Fe1—C9—C10 | 118.82 |
C6—Fe1—C1—C2 | 80.39 | C6—Fe1—C10—C9 | −119.54 |
C7—Fe1—C1—C2 | 39.74 | C2—Fe1—C8—C7 | 52.27 |
C9—Fe1—C1—C2 | 167.27 | C4—Fe1—C6—C10 | −152.71 |
C10—Fe1—C1—C2 | 124.03 | C5—Fe1—C6—C10 | 43.99 |
C2—Fe1—C1—C5 | 119.35 | C1—Fe1—C10—C6 | −118.05 |
C3—Fe1—C1—C5 | 81.64 | C2—Fe1—C10—C6 | −74.56 |
C4—Fe1—C1—C5 | 38.05 | C9—Fe1—C6—C10 | −37.41 |
C6—Fe1—C1—C5 | −160.26 | C7—Fe1—C10—C6 | 37.73 |
C7—Fe1—C1—C5 | 159.09 | C8—Fe1—C10—C6 | 81.59 |
C9—Fe1—C1—C5 | −73.38 | C9—Fe1—C10—C6 | 119.54 |
C10—Fe1—C1—C5 | −116.63 | C1—Fe1—C10—C9 | 122.41 |
C2—Fe1—C1—C11 | −122.83 | C2—Fe1—C10—C9 | 165.9 |
C3—Fe1—C1—C11 | −160.53 | C4—Fe1—C10—C9 | 36.58 |
C4—Fe1—C1—C11 | 155.87 | C10—Fe1—C7—C8 | 81.39 |
C5—Fe1—C1—C11 | 117.83 | C5—Fe1—C10—C9 | 77.45 |
C6—Fe1—C1—C11 | −42.44 | C7—Fe1—C9—C10 | 81.15 |
C7—Fe1—C1—C11 | −83.08 | C8—Fe1—C10—C9 | −37.95 |
C9—Fe1—C1—C11 | 44.45 | C7—Fe1—C10—C9 | −81.81 |
C10—Fe1—C1—C11 | 1.2 | C1—Fe1—C9—C8 | 161.37 |
C6—Fe1—C8—C7 | −37.83 | C9—Fe1—C7—C6 | −81.12 |
C9—Fe1—C8—C7 | −119.11 | C10—Fe1—C7—C6 | −37.49 |
C10—Fe1—C8—C7 | −81.38 | C1—Fe1—C7—C8 | 174.81 |
C2—Fe1—C8—C9 | 171.38 | C2—Fe1—C7—C8 | −156.21 |
C3—Fe1—C8—C9 | −159.96 | C3—Fe1—C7—C8 | −115.04 |
C4—Fe1—C8—C9 | −118.88 | C4—Fe1—C7—C8 | −74.31 |
C5—Fe1—C8—C9 | −78.85 | C5—Fe1—C7—C8 | −45.05 |
C6—Fe1—C8—C9 | 81.28 | C6—Fe1—C7—C8 | 118.87 |
C7—Fe1—C8—C9 | 119.11 | C9—Fe1—C7—C8 | 37.75 |
C10—Fe1—C8—C9 | 37.72 | C4—Fe1—C9—C10 | −164.14 |
C10—Fe1—C5—C1 | 85.17 | C6—Fe1—C9—C10 | 37.33 |
C1—Fe1—C5—C4 | 118.43 | C4—Fe1—C10—C6 | 156.12 |
C2—Fe1—C5—C4 | 80.89 | C5—Fe1—C10—C6 | −163.01 |
C3—Fe1—C2—C1 | 119.14 | C7—Fe1—C9—C8 | −37.68 |
C4—Fe1—C2—C1 | 81.87 | C3—Fe1—C8—C7 | 80.94 |
C5—Fe1—C2—C1 | 38 | C4—Fe1—C8—C7 | 122.01 |
C6—Fe1—C2—C1 | −120.12 | C3—Fe1—C9—C8 | 42.69 |
C7—Fe1—C2—C1 | −163.52 | C4—Fe1—C9—C8 | 77.03 |
C8—Fe1—C2—C1 | 159.86 | C5—Fe1—C9—C10 | −121.32 |
C10—Fe1—C2—C1 | −78.73 | C5—Fe1—C9—C8 | 119.85 |
C1—Fe1—C2—C3 | −119.14 | C6—Fe1—C9—C8 | −81.50 |
C4—Fe1—C2—C3 | −37.28 | C10—Fe1—C9—C8 | −118.82 |
C5—Fe1—C2—C3 | −81.15 | C1—Fe1—C9—C10 | −79.81 |
C6—Fe1—C2—C3 | 120.74 | C3—Fe1—C9—C10 | 161.51 |
C7—Fe1—C2—C3 | 77.34 | C14—O2—C13—O1 | 179.94 |
C8—Fe1—C2—C3 | 40.72 | C13—O2—C14—C15 | 178.44 |
C10—Fe1—C2—C3 | 162.13 | C13—O2—C14—N1 | −1.05 |
C1—Fe1—C6—C10 | 83.36 | C14—O2—C13—C12 | 0.36 |
C2—Fe1—C6—C10 | 126.46 | C14—N1—C12—C13 | −0.93 |
C3—Fe1—C6—C10 | 169.34 | C12—N1—C14—O2 | 1.25 |
C1—Fe1—C3—C2 | 37.8 | C12—N1—C14—C15 | −178.17 |
C4—Fe1—C3—C2 | 119.73 | C14—N1—C12—C11 | 176.61 |
C5—Fe1—C3—C2 | 82.29 | C11—C1—C2—C3 | 177.97 |
C6—Fe1—C3—C2 | −79.80 | C5—C1—C2—Fe1 | −57.89 |
C7—Fe1—C3—C2 | −119.46 | Fe1—C1—C2—C3 | 59.02 |
C8—Fe1—C3—C2 | −161.12 | C11—C1—C2—Fe1 | 118.95 |
C9—Fe1—C3—C2 | 169 | C5—C1—C2—C3 | 1.13 |
C1—Fe1—C3—C4 | −81.93 | C2—C1—C11—C12 | 19.19 |
C2—Fe1—C3—C4 | −119.73 | C2—C1—C5—Fe1 | 58.65 |
C5—Fe1—C3—C4 | −37.44 | Fe1—C1—C11—C12 | 109.4 |
C6—Fe1—C3—C4 | 160.47 | Fe1—C1—C5—C4 | −59.99 |
C7—Fe1—C3—C4 | 120.81 | C11—C1—C5—Fe1 | −118.32 |
C8—Fe1—C3—C4 | 79.15 | C5—C1—C11—C12 | −164.49 |
C9—Fe1—C3—C4 | 49.27 | C11—C1—C5—C4 | −178.31 |
C4—Fe1—C7—C6 | 166.81 | C2—C1—C5—C4 | −1.34 |
C5—Fe1—C7—C6 | −163.92 | C1—C2—C3—C4 | −0.51 |
C8—Fe1—C7—C6 | −118.87 | C1—C2—C3—Fe1 | −59.45 |
C1—Fe1—C4—C3 | 81.37 | Fe1—C2—C3—C4 | 58.94 |
C2—Fe1—C4—C3 | 37.45 | C2—C3—C4—C5 | −0.34 |
C5—Fe1—C4—C3 | 119.88 | Fe1—C3—C4—C5 | 59.14 |
C6—Fe1—C4—C3 | −51.23 | C2—C3—C4—Fe1 | −59.48 |
C7—Fe1—C4—C3 | −76.08 | Fe1—C4—C5—C1 | 60.58 |
C8—Fe1—C4—C3 | −116.25 | C3—C4—C5—C1 | 1.04 |
C9—Fe1—C4—C3 | −157.09 | C3—C4—C5—Fe1 | −59.53 |
C10—Fe1—C4—C3 | 176.63 | C10—C6—C7—C8 | 0.21 |
C1—Fe1—C4—C5 | −38.50 | C7—C6—C10—C9 | −0.65 |
C2—Fe1—C4—C5 | −82.43 | Fe1—C6—C10—C9 | 59.08 |
C3—Fe1—C4—C5 | −119.88 | C10—C6—C7—Fe1 | 59.94 |
C6—Fe1—C4—C5 | −171.11 | C7—C6—C10—Fe1 | −59.73 |
C7—Fe1—C4—C5 | 164.04 | Fe1—C6—C7—C8 | −59.73 |
C8—Fe1—C4—C5 | 123.87 | Fe1—C7—C8—C9 | −59.26 |
C9—Fe1—C4—C5 | 83.03 | C6—C7—C8—Fe1 | 59.56 |
C10—Fe1—C4—C5 | 56.75 | C6—C7—C8—C9 | 0.3 |
C5—Fe1—C8—C7 | 162.04 | Fe1—C8—C9—C10 | −60.02 |
C7—Fe1—C6—C10 | −119.17 | C7—C8—C9—C10 | −0.69 |
C8—Fe1—C6—C10 | −81.35 | C7—C8—C9—Fe1 | 59.32 |
C2—Fe1—C5—C1 | −37.54 | C8—C9—C10—Fe1 | 59.9 |
C3—Fe1—C5—C1 | −81.26 | Fe1—C9—C10—C6 | −59.07 |
C4—Fe1—C5—C1 | −118.43 | C8—C9—C10—C6 | 0.83 |
C6—Fe1—C5—C1 | 52.64 | C1—C11—C12—C13 | −179.36 |
C7—Fe1—C5—C1 | −158.20 | C1—C11—C12—N1 | 3.44 |
C8—Fe1—C5—C1 | 168.74 | C11—C12—C13—O2 | −177.35 |
C9—Fe1—C5—C1 | 126.69 | N1—C12—C13—O1 | −179.18 |
C1—Fe1—C7—C6 | 55.94 | N1—C12—C13—O2 | 0.33 |
C2—Fe1—C7—C6 | 84.92 | C11—C12—C13—O1 | 3.15 |
C3—Fe1—C7—C6 | 126.09 | O2—C14—C15—C16 | −173.83 |
C3—Fe1—C5—C4 | 37.17 | O2—C14—C15—C20 | 5.45 |
C6—Fe1—C5—C4 | 171.07 | N1—C14—C15—C16 | 5.58 |
C7—Fe1—C5—C4 | −39.76 | N1—C14—C15—C20 | −175.14 |
C8—Fe1—C5—C4 | −72.83 | C14—C15—C16—C17 | 179.17 |
C9—Fe1—C5—C4 | −114.87 | C20—C15—C16—C17 | −0.13 |
C10—Fe1—C5—C4 | −156.39 | C14—C15—C20—C19 | −179.68 |
C1—Fe1—C6—C7 | −157.47 | C16—C15—C20—C19 | −0.40 |
C2—Fe1—C6—C7 | −114.37 | C15—C16—C17—C18 | 0.45 |
C3—Fe1—C6—C7 | −71.48 | C16—C17—C18—C19 | −0.23 |
C4—Fe1—C6—C7 | −33.54 | C17—C18—C19—C20 | −0.30 |
C5—Fe1—C6—C7 | 163.16 | C18—C19—C20—C15 | 0.61 |
C8—Fe1—C6—C7 | 37.83 | | |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) −x, −y+1, −z; (iv) −x, −y, −z. |
(18) bis((mu!2$-Chloro)-diaqua-(2,4-pentanedione-O,
O')-magnesium) diaqua-bis(2,4-pe ntanedione-O,
O')-magnesium dichloride
top
Crystal data top
C10H24Cl2Mg2O8·C10H20MgO6·4(Cl) | Z = 2 |
Mr = 794.18 | F(000) = 740 |
Orthorhombic, Pmna | Dx = 1.315 Mg m−3 |
Hall symbol: -P 2ac 2 | Mo Kα radiation, λ = 0.71070 Å |
a = 13.303 (3) Å | µ = 0.55 mm−1 |
b = 7.835 (2) Å | T = 0 K |
c = 18.169 (4) Å | × × mm |
V = 1893.7 (8) Å3 | |
Data collection top
Radiation source: fine-focus sealed tube | θmax = 37.8°, θmin = 1.9° |
16258 measured reflections | h = −13→13 |
2204 independent reflections | k = −8→8 |
1626 reflections with I > 2σ(I) | l = −18→18 |
Rint = 0.274 | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.129 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.473 | H atoms treated by a mixture of independent and constrained refinement |
S = 2.65 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
2204 reflections | (Δ/σ)max = 0.593 |
54 parameters | Extinction correction: nne |
0 restraints | |
Crystal data top
C10H24Cl2Mg2O8·C10H20MgO6·4(Cl) | V = 1893.7 (8) Å3 |
Mr = 794.18 | Z = 2 |
Orthorhombic, Pmna | Mo Kα radiation |
a = 13.303 (3) Å | µ = 0.55 mm−1 |
b = 7.835 (2) Å | T = 0 K |
c = 18.169 (4) Å | × × mm |
Data collection top
16258 measured reflections | 1626 reflections with I > 2σ(I) |
2204 independent reflections | Rint = 0.274 |
Refinement top
R[F2 > 2σ(F2)] = 0.129 | 54 parameters |
wR(F2) = 0.473 | 0 restraints |
S = 2.65 | H atoms treated by a mixture of independent and constrained refinement |
2204 reflections | (Δ/σ)max = 0.593 |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is nt relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mg2 | 0.5 | 0.5 | 0 | 0.02* | |
O5 | 0.5 | 0.7546 | 0.0239 | 0.02* | |
O6 | 0.3832 | 0.4603 | 0.0739 | 0.02* | |
C6 | 0.29165 | 0.45435 | 0.0674 | 0.02* | |
C7 | 0.2381 | 0.5 | 0 | 0.02* | |
C9 | 0.22835 | 0.406 | 0.13295 | 0.02* | |
Cl1 | 0 | 1.20660 | 0.0285 | 0.02* | |
Mg1 | 0 | 0.9315 | 0.09570 | 0.02* | |
O1 | 0.15235 | 0.91845 | 0.1063 | 0.02* | |
O3 | 0 | 0.6986 | 0.15360 | 0.02* | |
O4 | 0 | 1.0335 | 0.2026 | 0.02* | |
C1 | 0 | 0.66110 | 0.2177 | 0.02* | |
C2 | 0 | 0.7871 | 0.279 | 0.02* | |
C3 | 0 | 0.9693 | 0.2639 | 0.02* | |
C4 | 0 | 0.4783 | 0.2428 | 0.02* | |
C5 | 0 | 1.0782 | 0.3334 | 0.02* | |
Cl2 | 0.25 | 0.79650 | 0.25 | 0.02* | |
Cl3 | 0.32480 | 0 | 0 | 0.02* | |
Geometric parameters (Å, º) top
Cl1—Mg1 | 2.4772 (6) | O3—C1 | 1.2011 (3) |
Mg2—O6 | 2.077 | O4—C3 | 1.2221 (3) |
Mg2—O5i | 2.0415 (5) | C6—C9 | 1.507 |
Mg2—O5 | 2.0415 (5) | C6—C7 | 1.4612 |
Mg1—O1 | 2.0384 | C1—C2 | 1.4883 (4) |
Mg1—O3 | 2.1063 (5) | C1—C4 | 1.5031 (4) |
Mg1—O4 | 2.1003 (5) | C2—C3 | 1.4537 (4) |
O6—C6 | 1.2245 | C3—C5 | 1.5240 (4) |
| | | |
Cl1···Cl1ii | 3.3990 (9) | O1···Cl1ii | 3.3266 |
Cl1···Mg1ii | 2.5026 (6) | O1···Cl3i | 3.0662 |
Cl1···O1ii | 3.3266 | O1···O3 | 2.7952 |
Cl1···O3ii | 3.3909 (9) | O3···O1 | 2.7952 |
Cl1···Cl1iii | 3.3990 (9) | O3···Cl1iii | 3.3909 (9) |
Cl1···Mg1iii | 2.5026 (6) | O3···Cl1ii | 3.3909 (9) |
Cl1···O1iii | 3.3266 | O3···O4 | 2.7709 (7) |
Cl1···O3iii | 3.3909 (9) | O3···O1iv | 2.7952 |
Cl1···O1iv | 3.347 | O4···O3 | 2.7709 (7) |
Cl1···O1 | 3.347 | O4···O1 | 2.8252 |
Cl1···O4 | 3.4417 (9) | O4···O1iv | 2.8252 |
Cl2···C3v | 3.5996 (9) | O4···Cl1 | 3.4417 (9) |
Cl2···C3 | 3.5996 (9) | O5···O6x | 2.8994 |
Cl2···C1 | 3.5398 (9) | O5···O6i | 2.8994 |
Cl2···C2 | 3.3680 (9) | O5···Cl3x | 3.0525 (8) |
Cl2···C1 | 3.5398 (9) | O5···Cl3ix | 3.0525 (8) |
Cl2···C2 | 3.3680 (9) | O5···O6 | 2.9251 |
Cl2···C3 | 3.5996 (9) | O5···Cl3i | 3.0525 (8) |
Cl2···O1vi | 3.0687 | O5···O6xi | 2.9251 |
Cl2···C1vi | 3.5398 (9) | O5···Cl3xii | 3.0525 (8) |
Cl2···C2vi | 3.3680 (9) | O6···O6xi | 3.1076 |
Cl2···C3vi | 3.5996 (9) | O6···O5i | 2.8994 |
Cl2···C1v | 3.5398 (9) | O6···O5 | 2.9251 |
Cl2···C2v | 3.3680 (9) | O6···O5i | 2.8994 |
Cl2···O1 | 3.0687 | O6···O6i | 2.7565 |
Cl3···O1i | 3.0662 | C1···Cl2iv | 3.5398 (9) |
Cl3···O5i | 3.0525 (8) | C1···Cl2 | 3.5398 (9) |
Cl3···O5i | 3.0525 (8) | C1···Cl2vi | 3.5398 (9) |
Cl3···O5vii | 3.0525 (8) | C1···Cl2xiii | 3.5398 (9) |
Cl3···O5viii | 3.0525 (8) | C2···Cl2xiii | 3.3680 (9) |
Cl3···O1viii | 3.0662 | C2···Cl2iv | 3.3680 (9) |
Mg1···Cl1ii | 2.5026 (6) | C2···Cl2vi | 3.3680 (9) |
Mg1···Cl1iii | 2.5026 (6) | C2···Cl2 | 3.3680 (9) |
Mg1···Mg1iii | 3.6394 (9) | C3···Cl2 | 3.5996 (9) |
Mg1···Mg1ii | 3.6394 (9) | C3···Cl2xiii | 3.5996 (9) |
O1···Cl2 | 3.0687 | C3···Cl2iv | 3.5996 (9) |
O1···Cl1 | 3.347 | C3···Cl2vi | 3.5996 (9) |
O1···O4 | 2.8252 | C4···C5xiv | 3.5407 (9) |
O1···Cl3ix | 3.0662 | C4···C5viii | 3.5407 (9) |
O1···Cl1iii | 3.3266 | C5···C4xv | 3.5407 (9) |
O1···Cl2vi | 3.0687 | C5···C4ix | 3.5407 (9) |
| | | |
O5—Mg2—O6 | 90.51 | Cl1—Mg1—O1 | 95.18 |
O5—Mg2—O5i | 180 | Cl1—Mg1—O3 | 179.57 |
O5—Mg2—O6i | 89.49 | O1iv—Mg1—O4 | 86.08 |
O5—Mg2—O6x | 89.49 | O3—Mg1—O4 | 82.4 |
O5—Mg2—O6xi | 90.51 | O1iv—Mg1—O3 | 84.8 |
O5i—Mg2—O6 | 89.49 | Mg2—O6—C6 | 133.43 |
O6—Mg2—O6i | 83.15 | Mg1—O3—C1 | 134.12 |
O6—Mg2—O6x | 180 | Mg1—O4—C3 | 133.33 |
O6—Mg2—O6xi | 96.85 | C7—C6—C9 | 116.84 |
O5i—Mg2—O6i | 90.51 | O6—C6—C9 | 119.28 |
O5i—Mg2—O6x | 90.51 | O6—C6—C7 | 123.81 |
O5i—Mg2—O6xi | 89.49 | C6—C7—C6i | 121.64 |
O6i—Mg2—O6x | 96.85 | O3—C1—C2 | 124.29 |
O6i—Mg2—O6xi | 180 | O3—C1—C4 | 121.82 |
O6x—Mg2—O6xi | 83.15 | C2—C1—C4 | 113.89 |
Cl1—Mg1—O4 | 97.16 | C1—C2—C3 | 120.67 |
Cl1—Mg1—O1iv | 95.18 | O4—C3—C2 | 125.18 |
O1—Mg1—O3 | 84.8 | O4—C3—C5 | 121.65 |
O1—Mg1—O4 | 86.08 | C2—C3—C5 | 113.17 |
O1—Mg1—O1iv | 167.72 | | |
| | | |
O5—Mg2—O6—C6 | 94.08 | Mg1—O3—C1—C4 | 180 |
O5i—Mg2—O6—C6 | −85.92 | Mg1—O3—C1—C2 | 0 |
O6i—Mg2—O6—C6 | 4.65 | Mg1—O4—C3—C5 | −180.00 |
O6xi—Mg2—O6—C6 | −175.35 | Mg1—O4—C3—C2 | 0 |
O1—Mg1—O4—C3 | −85.27 | C9—C6—C7—C6i | −178.73 |
O3—Mg1—O4—C3 | 0 | O6—C6—C7—C6i | 4.39 |
O4—Mg1—O3—C1 | 0 | O3—C1—C2—C3 | 0 |
Cl1—Mg1—O4—C3 | 180 | C4—C1—C2—C3 | −180.00 |
O1—Mg1—O3—C1 | 86.73 | C1—C2—C3—C5 | 180 |
Mg2—O6—C6—C9 | 174.32 | C1—C2—C3—O4 | 0 |
Mg2—O6—C6—C7 | −8.88 | | |
Symmetry codes: (i) x, −y+1, −z; (ii) x, −y+2, −z; (iii) −x, −y+2, −z; (iv) −x, y, z; (v) x+1/2, y, −z+1/2; (vi) −x+1/2, y, −z+1/2; (vii) −x+1, y−1, z; (viii) x, y−1, z; (ix) x, y+1, z; (x) −x+1, −y+1, −z; (xi) −x+1, y, z; (xii) −x+1, y+1, z; (xiii) x−1/2, y, −z+1/2; (xiv) −x, y−1, z; (xv) −x, y+1, z. |
(19) tris((mu!2$-Cyan)-tetracarbonyl-rhenium)
top
Crystal data top
C12N6O12Re3 | Z = 4 |
Mr = 978.81 | F(000) = 1740 |
Orthorhombic, Pnma | Dx = 2.820 Mg m−3 |
Hall symbol: -P 2ac 2n | Mo K\a radiation, λ = 0.71073 Å |
a = 20.639 (3) Å | µ = 15.78 mm−1 |
b = 16.657 (3) Å | T = 0 K |
c = 6.705 (3) Å | × × mm |
V = 2305.1 (12) Å3 | |
Crystal data top
C12N6O12Re3 | V = 2305.1 (12) Å3 |
Mr = 978.81 | Z = 4 |
Orthorhombic, Pnma | Mo K\a radiation |
a = 20.639 (3) Å | µ = 15.78 mm−1 |
b = 16.657 (3) Å | T = 0 K |
c = 6.705 (3) Å | × × mm |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Re1 | 0.12255 | 0.09275 | 0.51490 | 0.02* | |
Re2 | −0.07920 | 0.25 | 0.2172 | 0.02* | |
O1 | 0.1973 | 0.13705 | 0.1247 | 0.02* | |
O2 | 0.04935 | 0.0573 | 0.9156 | 0.02* | |
O3 | 0.24705 | 0.0414 | 0.72845 | 0.02* | |
O4 | 0.09845 | −0.07660 | 0.34295 | 0.02* | |
O5 | −0.00740 | 0.25 | −0.20150 | 0.02* | |
O6 | −0.17165 | 0.1146 | 0.0793 | 0.02* | |
O7 | −0.15240 | 0.25 | 0.62410 | 0.02* | |
N1 | 0.0301 | 0.1348 | 0.3735 | 0.02* | |
N3 | 0.1347 | 0.215 | 0.5818 | 0.02* | |
N13 | −0.00600 | 0.1711 | 0.3139 | 0.02* | |
C1 | 0.1707 | 0.12375 | 0.26575 | 0.02* | |
C2 | 0.07370 | 0.0697 | 0.75875 | 0.02* | |
C3 | 0.20365 | 0.06195 | 0.6473 | 0.02* | |
C4 | 0.1073 | −0.01415 | 0.4164 | 0.02* | |
C5 | −0.03500 | 0.25 | −0.04670 | 0.02* | |
C6 | −0.13530 | 0.16535 | 0.1311 | 0.02* | |
C7 | −0.12430 | 0.25 | 0.4866 | 0.02* | |
Geometric parameters (Å, º) top
Re1—N1 | 2.2428 | O1—C1 | 1.1158 |
Re1—N3 | 2.1002 | O2—C2 | 1.1837 |
Re1—C1 | 2.0112 | O3—C3 | 1.1025 |
Re1—C2 | 1.9589 | O4—C4 | 1.1653 |
Re1—C3 | 1.9629 | O5—C5 | 1.1840 (5) |
Re1—C4 | 1.9251 | O6—C6 | 1.1824 |
Re2—N13 | 2.1048 | O7—C7 | 1.0892 (5) |
Re2—C5 | 1.9908 (9) | N1—N13 | 1.0394 |
Re2—C6 | 1.9136 | N3—N3i | 1.166 |
Re2—C7 | 2.0321 (9) | | |
| | | |
O2···O2ii | 3.0124 | O7···C5x | 3.2777 (15) |
O3···C1iii | 3.2422 | O7···O4xi | 3.1034 |
O3···C4iii | 3.291 | O7···O4vi | 3.1034 |
O3···O6iv | 2.9258 | O7···O5xii | 3.2130 (14) |
O4···O7v | 3.1034 | O7···C5xii | 3.2777 (15) |
O4···C7v | 3.1517 | C1···O3xiii | 3.2422 |
O4···O7vi | 3.1034 | C1···O6iv | 3.419 |
O4···C7vi | 3.1517 | C3···O6iv | 3.1147 |
O5···O7vii | 3.2130 (14) | C4···O3xiii | 3.291 |
O5···C7vii | 3.1929 (14) | C5···O7vii | 3.2777 (15) |
O5···O7viii | 3.2130 (14) | C5···O7viii | 3.2777 (15) |
O5···C7viii | 3.1929 (14) | C7···O5x | 3.1929 (14) |
O6···O3ix | 2.9258 | C7···O4xi | 3.1517 |
O6···C1ix | 3.419 | C7···O4vi | 3.1517 |
O6···C3ix | 3.1147 | C7···O5xii | 3.1929 (14) |
O7···O5x | 3.2130 (14) | | |
| | | |
N1—Re1—N3 | 83.63 | C5—Re2—C6 | 90.52 |
N1—Re1—C1 | 89.37 | C5—Re2—C7 | 179.97 |
N1—Re1—C2 | 88.63 | N13i—Re2—C5 | 86.84 |
N1—Re1—C3 | 176.62 | C5—Re2—C6i | 90.52 |
N1—Re1—C4 | 90.27 | C6—Re2—C7 | 89.49 |
N3—Re1—C1 | 82.5 | N13i—Re2—C6 | 170.86 |
N3—Re1—C2 | 94.2 | C6—Re2—C6i | 94.92 |
N3—Re1—C3 | 93.15 | N13i—Re2—C7 | 93.15 |
N3—Re1—C4 | 171.75 | C6i—Re2—C7 | 89.49 |
C1—Re1—C2 | 176.32 | N13i—Re2—C6i | 93.85 |
C1—Re1—C3 | 91.23 | Re1—N1—N13 | 162.55 |
C1—Re1—C4 | 91.91 | Re1—N3—N3i | 165.84 |
C2—Re1—C3 | 90.58 | Re2—N13—N1 | 174.98 |
C2—Re1—C4 | 91.2 | Re1—C1—O1 | 176.52 |
C3—Re1—C4 | 93.03 | Re1—C2—O2 | 173.86 |
N13—Re2—C5 | 86.84 | Re1—C3—O3 | 175.66 |
N13—Re2—C6 | 93.85 | Re1—C4—O4 | 175.06 |
N13—Re2—C7 | 93.15 | Re2—C5—O5 | 178.51 |
N13—Re2—N13i | 77.28 | Re2—C6—O6 | 177.85 |
N13—Re2—C6i | 170.86 | Re2—C7—O7 | 175.09 |
Symmetry codes: (i) x, −y+1/2, z; (ii) −x, −y, −z+2; (iii) −x+1/2, −y, z+1/2; (iv) x+1/2, y, −z+1/2; (v) −x, y−1/2, −z+1; (vi) −x, −y, −z+1; (vii) x, y, z−1; (viii) x, −y+1/2, z−1; (ix) x−1/2, y, −z+1/2; (x) x, y, z+1; (xi) −x, y+1/2, −z+1; (xii) x, −y+1/2, z+1; (xiii) −x+1/2, −y, z−1/2. |
(20) 2-(4'-Cyanphenylthio)-5-methylthiadiazole
top
Crystal data top
C10H7N3S2 | γ = 90° |
Mr = 233.33 | V = 524.1 (2) Å3 |
Monclinic, P21/m | Z = 2 |
Hall symbol: -P 2yb | F(000) = 240 |
a = 5.628 (1) Å | Dx = 1.479 Mg m−3 |
b = 7.207 (2) Å | Mo K\a radiation, λ = 0.71073 Å |
c = 13.126 (2) Å | µ = 0.47 mm−1 |
α = 90° | T = 0 K |
β = 100.12 (6)° | × × mm |
Crystal data top
C10H7N3S2 | γ = 90° |
Mr = 233.33 | V = 524.1 (2) Å3 |
Monclinic, P21/m | Z = 2 |
a = 5.628 (1) Å | Mo K\a radiation |
b = 7.207 (2) Å | µ = 0.47 mm−1 |
c = 13.126 (2) Å | T = 0 K |
α = 90° | × × mm |
β = 100.12 (6)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
S1 | 0.41806 | 0.25 | 0.18596 | 0.05* | |
S2 | 0.79678 | 0.25 | 0.04157 | 0.05* | |
N1 | 0.3413 | 0.25 | −0.01690 | 0.05* | |
N2 | 0.4406 | 0.25 | −0.10660 | 0.05* | |
N3 | 1.5272 | 0.25 | 0.54220 | 0.05* | |
C1 | 0.5051 | 0.25 | 0.0643 | 0.05* | |
C2 | 0.6743 | 0.25 | −0.08820 | 0.05* | |
C3 | 0.8246 | 0.25 | −0.17030 | 0.05* | |
C4 | 0.70310 | 0.25 | 0.2703 | 0.05* | |
C5 | 0.8097 | 0.0831 | 0.30425 | 0.05* | |
C6 | 1.0244 | 0.0828 | 0.37345 | 0.05* | |
C7 | 1.1292 | 0.25 | 0.4088 | 0.05* | |
C10 | 1.3526 | 0.25 | 0.4826 | 0.05* | |
H1 | 0.9921 | 0.25 | −0.13910 | 0.05* | |
H2 | 0.78945 | 0.14135 | −0.21250 | 0.05* | |
H4 | 0.73695 | −0.02825 | 0.2806 | 0.05* | |
H5 | 1.098 | −0.02875 | 0.39625 | 0.05* | |
Geometric parameters (Å, º) top
S1—C1 | 1.7507 (5) | C4—C5 | 1.3825 |
S1—C4 | 1.7818 (5) | C5—C6 | 1.3782 |
S2—C1 | 1.7193 (5) | C6—C7 | 1.3853 |
S2—C2 | 1.7216 (5) | C7—C10 | 1.4461 (4) |
N1—N2 | 1.3892 (4) | C3—H1 | 0.9595 |
N1—C1 | 1.2808 (4) | C3—H2 | 0.9595 |
N2—C2 | 1.2948 (4) | C5—H4 | 0.9292 |
N3—C10 | 1.1434 (3) | C6—H5 | 0.9295 |
C2—C3 | 1.4823 (4) | | |
| | | |
S1···S2i | 3.6728 (10) | N2···H1ii | 2.4849 |
S1···C7i | 3.5874 (10) | N3···H5viii | 2.6544 |
S1···C7ii | 3.5874 (10) | N3···H5ix | 2.6544 |
S1···S2ii | 3.6728 (10) | C3···N1iv | 3.2331 (9) |
S2···N1iii | 3.2874 (9) | C3···N2iv | 3.4204 (9) |
S2···S1iii | 3.6728 (10) | C3···N1iii | 3.2331 (9) |
S2···S1iv | 3.6728 (10) | C3···N2iii | 3.4204 (9) |
S2···N1iv | 3.2874 (9) | C5···S2 | 3.6404 |
S2···C5 | 3.6404 | C6···C6x | 3.5857 |
S2···C5v | 3.6404 | C7···S1iv | 3.5874 (10) |
S1···H2vi | 3.0957 | C7···S1iii | 3.5874 (10) |
S1···H2vii | 3.0957 | C6···H2xi | 2.9914 |
N1···S2i | 3.2874 (9) | H1···N1iv | 2.3081 |
N1···C3i | 3.2331 (9) | H1···N2iv | 2.4849 |
N1···S2ii | 3.2874 (9) | H1···N1iii | 2.3081 |
N1···C3ii | 3.2331 (9) | H1···N2iii | 2.4849 |
N2···C3i | 3.4204 (9) | H2···S1xii | 3.0957 |
N2···C3ii | 3.4204 (9) | H2···S1vii | 3.0957 |
N1···H1i | 2.3081 | H2···C6xi | 2.9914 |
N1···H1ii | 2.3081 | H4···N2xii | 2.8226 |
N2···H4vi | 2.8226 | H4···N2vii | 2.8226 |
N2···H4vii | 2.8226 | H5···N3xiii | 2.6544 |
N2···H1i | 2.4849 | H5···N3ix | 2.6544 |
| | | |
C1—S1—C4 | 101.60 (6) | C6—C7—C10 | 119.56 |
C1—S2—C2 | 86.74 (6) | C6—C7—C6v | 120.88 |
N2—N1—C1 | 111.55 (6) | C6v—C7—C10 | 119.56 |
N1—N2—C2 | 112.87 (6) | N3—C10—C7 | 178.92 (6) |
S1—C1—S2 | 125.95 (6) | C2—C3—H1 | 109.45 |
S1—C1—N1 | 118.89 (6) | C2—C3—H2 | 109.49 |
S2—C1—N1 | 115.16 (6) | C2—C3—H2v | 109.49 |
S2—C2—N2 | 113.67 (6) | H1—C3—H2 | 109.5 |
S2—C2—C3 | 122.61 (6) | H1—C3—H2v | 109.5 |
N2—C2—C3 | 123.72 (6) | H2—C3—H2v | 109.39 |
S1—C4—C5 | 119.51 | C4—C5—H4 | 120.2 |
S1—C4—C5v | 119.51 | C6—C5—H4 | 120.18 |
C5—C4—C5v | 120.92 | C5—C6—H5 | 120.2 |
C4—C5—C6 | 119.63 | C7—C6—H5 | 120.34 |
C5—C6—C7 | 119.46 | | |
| | | |
C4—S1—C1—S2 | 0.00 (6) | N2—N1—C1—S1 | 180.00 (6) |
C4—S1—C1—N1 | 180.00 (6) | N1—N2—C2—S2 | 0.00 (6) |
C1—S1—C4—C5 | −91.33 | N1—N2—C2—C3 | 180.00 (6) |
C1—S2—C2—N2 | 0.00 (6) | S1—C4—C5—C6 | −176.85 |
C2—S2—C1—S1 | 180.00 (6) | C5v—C4—C5—C6 | 0.45 |
C1—S2—C2—C3 | 180.00 (6) | C4—C5—C6—C7 | 0.63 |
C2—S2—C1—N1 | 0.00 (6) | C5—C6—C7—C10 | 179.08 |
N2—N1—C1—S2 | 0.00 (6) | C5—C6—C7—C6v | −1.71 |
C1—N1—N2—C2 | 0.00 (6) | | |
Symmetry codes: (i) x−1, y, z; (ii) x−1, −y+1/2, z; (iii) x+1, −y+1/2, z; (iv) x+1, y, z; (v) x, −y+1/2, z; (vi) −x+1, y+1/2, −z; (vii) −x+1, −y, −z; (viii) −x+3, y+1/2, −z+1; (ix) −x+3, −y, −z+1; (x) −x+2, −y, −z+1; (xi) −x+2, −y, −z; (xii) −x+1, y−1/2, −z; (xiii) −x+3, y−1/2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H1···N1iv | 0.96 | 2.31 | 3.2331 (9) | 162 |
C3—H1···N2iv | 0.96 | 2.48 | 3.4204 (9) | 165 |
C3—H1···N1iii | 0.96 | 2.31 | 3.2331 (9) | 162 |
C3—H1···N2iii | 0.96 | 2.48 | 3.4204 (9) | 165 |
Symmetry codes: (iii) x+1, −y+1/2, z; (iv) x+1, y, z. |
(21)
trans-bis(mu!2$-Chloro)-dichloro-dicarbonyl-di-platinum(ii)
top
Crystal data top
C2Cl4O2Pt2 | Z = 2 |
Mr = 587.98 | F(000) = 504 |
Tetragonal, P42/m | Dx = 4.430 Mg m−3 |
Hall symbol: -P 4c | Mo K\a radiation, λ = 0.71073 Å |
a = 11.183 (3) Å | µ = 32.85 mm−1 |
c = 3.525 (2) Å | T = 0 K |
V = 440.8 (3) Å3 | × × mm |
Crystal data top
C2Cl4O2Pt2 | Z = 2 |
Mr = 587.98 | Mo K\a radiation |
Tetragonal, P42/m | µ = 32.85 mm−1 |
a = 11.183 (3) Å | T = 0 K |
c = 3.525 (2) Å | × × mm |
V = 440.8 (3) Å3 | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pt1 | 0.3915 | 0.10905 | 0 | 0.02* | |
Cl1 | 0.59570 | 0.1045 | 0 | 0.02* | |
Cl2 | 0.3826 | 0.2987 | 0 | 0.02* | |
O1 | 0.13 | 0.1 | 0 | 0.02* | |
C1 | 0.226 | 0.103 | 0 | 0.02* | |
Geometric parameters (Å, º) top
Pt1—Cl1 | 2.2841 (13) | Pt1—Cl1i | 2.3924 (14) |
Pt1—Cl2 | 2.1232 (12) | O1—C1 | 1.0741 (6) |
Pt1—C1 | 1.8520 (11) | | |
| | | |
Pt1···Pt1ii | 3.525 (2) | Cl2···Pt1ii | 4.115 (2) |
Pt1···Pt1iii | 3.525 (2) | Cl2···Pt1iii | 4.115 (2) |
Pt1···Cl1ii | 4.200 (2) | Cl2···Cl2ii | 3.525 (2) |
Pt1···Cl1iii | 4.200 (2) | Cl2···Cl2iii | 3.525 (2) |
Pt1···Cl2ii | 4.115 (2) | Cl2···Pt1iv | 4.115 (2) |
Pt1···Cl2iii | 4.115 (2) | Cl2···Pt1v | 4.115 (2) |
Pt1···C1ii | 3.982 (2) | Cl2···Cl2iv | 3.525 (2) |
Pt1···C1iii | 3.982 (2) | Cl2···Cl2v | 3.525 (2) |
Pt1···Pt1iv | 3.525 (2) | O1···O1vi | 3.1360 (18) |
Pt1···Pt1v | 3.525 (2) | O1···O1vii | 3.1360 (18) |
Pt1···Cl1iv | 4.200 (2) | O1···O1viii | 3.1360 (18) |
Pt1···Cl1v | 4.200 (2) | O1···O1ix | 3.1360 (18) |
Pt1···Cl2iv | 4.115 (2) | O1···O1x | 3.1360 (18) |
Pt1···Cl2v | 4.115 (2) | O1···O1xi | 3.1360 (18) |
Pt1···C1iv | 3.982 (2) | O1···O1xii | 3.1360 (18) |
Pt1···C1v | 3.982 (2) | O1···O1xiii | 3.1360 (18) |
Cl1···Pt1ii | 4.200 (2) | C1···Pt1ii | 3.982 (2) |
Cl1···Pt1iii | 4.200 (2) | C1···Pt1iii | 3.982 (2) |
Cl1···Cl1ii | 3.525 (2) | C1···C1ii | 3.525 (2) |
Cl1···Cl1iii | 3.525 (2) | C1···C1iii | 3.525 (2) |
Cl1···Pt1iv | 4.200 (2) | C1···Pt1iv | 3.982 (2) |
Cl1···Pt1v | 4.200 (2) | C1···Pt1v | 3.982 (2) |
Cl1···Cl1iv | 3.525 (2) | C1···C1iv | 3.525 (2) |
Cl1···Cl1v | 3.525 (2) | C1···C1v | 3.525 (2) |
| | | |
Cl1—Pt1—Cl2 | 93.96 | Cl1i—Pt1—Cl2 | 179.26 |
Cl1—Pt1—C1 | 176.63 | Cl1i—Pt1—C1 | 91.34 |
Cl1—Pt1—Cl1i | 85.29 | Pt1—Cl1—Pt1i | 94.71 |
Cl2—Pt1—C1 | 89.41 | Pt1—C1—O1 | 179.7 |
Symmetry codes: (i) −x+1, −y, z; (ii) x, y, z−1; (iii) x, y, z+1; (iv) x, y, −z−1; (v) x, y, −z+1; (vi) −y, x, z−1/2; (vii) −y, x, z+1/2; (viii) y, −x, z−1/2; (ix) y, −x, z+1/2; (x) y, −x, −z−1/2; (xi) y, −x, −z+1/2; (xii) −y, x, −z−1/2; (xiii) −y, x, −z+1/2. |
(22) Dihydro-1
H-pyrrolizine-3,5(2
H,6H)-dione
top
Crystal data top
C7H9NO2 | γ = 90° |
Mr = 139.15 | V = 340.0 (3) Å3 |
Monclinic, P21/m | Z = 2 |
Hall symbol: -P 2yb | F(000) = 148 |
a = 7.110 (4) Å | Dx = 1.271 Mg m−3 |
b = 6.993 (4) Å | Mo K\a radiation, λ = 0.71073 Å |
c = 7.678 (4) Å | µ = 0.10 mm−1 |
α = 90° | T = 0 K |
β = 117.04 (4)° | × × mm |
Crystal data top
C7H9NO2 | γ = 90° |
Mr = 139.15 | V = 340.0 (3) Å3 |
Monclinic, P21/m | Z = 2 |
a = 7.110 (4) Å | Mo K\a radiation |
b = 6.993 (4) Å | µ = 0.10 mm−1 |
c = 7.678 (4) Å | T = 0 K |
α = 90° | × × mm |
β = 117.04 (4)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
O1 | 1.2838 | 0.25 | 0.7036 | 0.05* | |
O2 | 1.0045 | 0.25 | 0.2625 | 0.05* | |
N1 | 0.9252 | 0.25 | 0.51920 | 0.05* | |
C2 | 1.0457 | 0.25 | 0.8528 | 0.05* | |
C3 | 1.1091 | 0.25 | 0.6901 | 0.05* | |
C4 | 0.8777 | 0.25 | 0.3245 | 0.05* | |
C5 | 0.6408 | 0.25 | 0.2127 | 0.05* | |
C1 | 0.8092 | 0.2327 | 0.74910 | 0.05* | 0.25 |
C1' | 0.8092 | 0.2673 | 0.74910 | 0.05* | 0.25 |
C6 | 0.5716 | 0.2283 | 0.3694 | 0.05* | 0.25 |
C6' | 0.5716 | 0.2717 | 0.3694 | 0.05* | 0.25 |
C7 | 0.73510 | 0.29140 | 0.54940 | 0.05* | 0.25 |
C7' | 0.73510 | 0.2086 | 0.54940 | 0.05* | 0.25 |
Geometric parameters (Å, º) top
O1—C3 | 1.1986 (7) | C1'—C7' | 1.4362 |
O2—C4 | 1.1957 (7) | C2—C3 | 1.5085 (9) |
N1—C3 | 1.3680 (8) | C4—C5 | 1.5031 (9) |
N1—C4 | 1.3747 (8) | C5—C6 | 1.5003 |
N1—C7 | 1.4998 | C5—C6' | 1.5003 |
N1—C7' | 1.4998 | C6—C6' | 0.3035 |
C1—C7' | 1.3865 | C6—C7 | 1.4126 |
C1—C2 | 1.5029 | C6—C7' | 1.3489 |
C1—C1' | 0.242 | C6'—C7 | 1.3489 |
C1—C7 | 1.4362 | C6'—C7' | 1.4126 |
C1'—C2 | 1.5029 | C7—C7' | 0.579 |
C1'—C7 | 1.3865 | | |
| | | |
O1···O2 | 3.0494 (17) | C3···C7'iii | 2.3896 |
O2···O1 | 3.0494 (17) | C4···C7'iii | 2.3844 |
O2···C2i | 3.2892 (19) | C4···C3ix | 3.501 (2) |
O2···C2ii | 3.2892 (19) | C4···C1iii | 3.5105 |
N1···C1iii | 2.2659 | C4···C1'iii | 3.5105 |
N1···C1'iii | 2.2659 | C4···C3vi | 3.501 (2) |
N1···C6iii | 2.2444 | C4···C3vii | 3.501 (2) |
N1···C6'iii | 2.2444 | C4···C3viii | 3.501 (2) |
N1···C7iii | 1.4998 | C4···C7iii | 2.3844 |
N1···C7'iii | 1.4998 | C4···C6iii | 2.3581 |
C1···C6iii | 2.6362 | C4···C6'iii | 2.3581 |
C1···C6'iii | 2.6222 | C5···C6iii | 1.5003 |
C1···C7iii | 1.3865 | C5···C6'iii | 1.5003 |
C1···C7'iii | 1.4362 | C5···C7iii | 2.375 |
C1···C1iii | 0.242 | C5···C7'iii | 2.375 |
C1'···C1'iii | 0.242 | C6···C1iii | 2.6362 |
C1'···C6'iii | 2.6362 | C6···C1'iii | 2.6222 |
C1'···C7iii | 1.4362 | C6···C6iii | 0.3035 |
C1'···C6iii | 2.6222 | C6···C7iii | 1.3489 |
C1'···C7'iii | 1.3865 | C6···C7'iii | 1.4126 |
C2···O2iv | 3.2892 (19) | C6'···C1iii | 2.6222 |
C2···C1iii | 1.5029 | C6'···C1'iii | 2.6362 |
C2···O2v | 3.2892 (19) | C6'···C6'iii | 0.3035 |
C2···C7iii | 2.3895 | C6'···C7iii | 1.4126 |
C2···C7'iii | 2.3895 | C6'···C7'iii | 1.3489 |
C2···C1'iii | 1.5029 | C7···C1iii | 1.3865 |
C3···C4vi | 3.501 (2) | C7···C1'iii | 1.4362 |
C3···C1iii | 2.3759 | C7···C6iii | 1.3489 |
C3···C1'iii | 2.3759 | C7···C6'iii | 1.4126 |
C3···C6iii | 3.4835 | C7···C7iii | 0.579 |
C3···C6'iii | 3.4835 | C7'···C1iii | 1.4362 |
C3···C7iii | 2.3896 | C7'···C1'iii | 1.3865 |
C3···C4vii | 3.501 (2) | C7'···C6iii | 1.4126 |
C3···C4viii | 3.501 (2) | C7'···C6'iii | 1.3489 |
C3···C4ix | 3.501 (2) | C7'···C7'iii | 0.579 |
| | | |
C3—N1—C4 | 134.29 (4) | C5—C6'—C6 | 84.19 |
C3—N1—C7 | 112.78 | C5—C6'—C7 | 112.82 |
C3—N1—C7' | 112.78 | C5—C6'—C7' | 109.21 |
C4—N1—C7 | 112.02 | C6—C6'—C7 | 95.86 |
C4—N1—C7' | 112.02 | C6—C6'—C7' | 71.8 |
C7—N1—C7' | 22.26 | C7—C6'—C7' | 24.06 |
C1'—C1—C7 | 73.39 | N1—C7—C1 | 101.01 |
C1'—C1—C7' | 96.98 | N1—C7—C1' | 103.38 |
C7—C1—C7' | 23.59 | N1—C7—C6 | 100.78 |
C2—C1—C7 | 108.76 | N1—C7—C6' | 103.85 |
C2—C1—C7' | 111.52 | N1—C7—C7' | 78.87 |
C1'—C1—C2 | 85.38 | C1—C7—C1' | 9.63 |
C1—C1'—C2 | 85.38 | C1—C7—C6 | 133.99 |
C2—C1'—C7 | 111.52 | C1—C7—C6' | 142.34 |
C7—C1'—C7' | 23.59 | C1—C7—C7' | 73.39 |
C2—C1'—C7' | 108.76 | C1'—C7—C6 | 140.71 |
C1—C1'—C7 | 96.98 | C1'—C7—C6' | 146.91 |
C1—C1'—C7' | 73.39 | C1'—C7—C7' | 83.02 |
C1'—C2—C3 | 104.17 | C6—C7—C6' | 12.34 |
C1—C2—C1' | 9.23 | C6—C7—C7' | 71.8 |
C1—C2—C3 | 104.17 | C6'—C7—C7' | 84.14 |
O1—C3—N1 | 125.73 (4) | N1—C7'—C1 | 103.38 |
O1—C3—C2 | 128.06 (4) | N1—C7'—C1' | 101.01 |
N1—C3—C2 | 106.21 (4) | N1—C7'—C6 | 103.85 |
O2—C4—N1 | 125.17 (4) | N1—C7'—C6' | 100.78 |
N1—C4—C5 | 106.17 (4) | N1—C7'—C7 | 78.87 |
O2—C4—C5 | 128.66 (4) | C1—C7'—C1' | 9.63 |
C4—C5—C6' | 103.47 | C1—C7'—C6 | 146.91 |
C6—C5—C6' | 11.61 | C1—C7'—C6' | 140.71 |
C4—C5—C6 | 103.47 | C1—C7'—C7 | 83.02 |
C5—C6—C6' | 84.19 | C1'—C7'—C6 | 142.34 |
C5—C6—C7 | 109.21 | C1'—C7'—C6' | 133.99 |
C5—C6—C7' | 112.82 | C1'—C7'—C7 | 73.39 |
C6'—C6—C7 | 71.8 | C6—C7'—C6' | 12.34 |
C6'—C6—C7' | 95.86 | C6—C7'—C7 | 84.14 |
C7—C6—C7' | 24.06 | C6'—C7'—C7 | 71.8 |
| | | |
C4—N1—C3—O1 | 0.00 (4) | C3—N1—C4—O2 | 0.00 (4) |
C4—N1—C3—C2 | 180.00 (4) | C3—N1—C4—C5 | 180.00 (4) |
Symmetry codes: (i) x, y, z−1; (ii) x, −y+1/2, z−1; (iii) x, −y+1/2, z; (iv) x, −y+1/2, z+1; (v) x, y, z+1; (vi) −x+2, −y+1, −z+1; (vii) −x+2, y−1/2, −z+1; (viii) −x+2, y+1/2, −z+1; (ix) −x+2, −y, −z+1. |
(23) Dichloro-(
S-methyl beta-
N-((2-hydroxyphenyl)ethylidene)dithiocarbazato)-bis (triphenylphosphine)-rhenium(v)
top
Crystal data top
C38H33Cl2N2P2ReS2 | γ = 90° |
Mr = 900.86 | V = 3660.5 (14) Å3 |
Monclinic, C2/c | Z = 4 |
Hall symbol: -C 2yc | F(000) = 1652 |
a = 17.514 (4) Å | Dx = 1.574 Mg m−3 |
b = 10.639 (2) Å | Mo Kα radiation, λ = 0.71070 Å |
c = 20.106 (4) Å | µ = 3.70 mm−1 |
α = 90° | T = 0 K |
β = 102.29 (3)° | × × mm |
Data collection top
Radiation source: fine-focus sealed tube | θmax = 41.8°, θmin = 2.1° |
17044 measured reflections | h = −18→18 |
4363 independent reflections | k = −11→11 |
4277 reflections with I > 2σ(I) | l = −20→20 |
Rint = 0.022 | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.049 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.259 | w = 1/[σ2(Fo2) + (0.2P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.18 | (Δ/σ)max = 0.946 |
4363 reflections | Δρmax = 2.01 e Å−3 |
105 parameters | Δρmin = −2.68 e Å−3 |
0 restraints | Extinction correction: nne |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
C38H33Cl2N2P2ReS2 | γ = 90° |
Mr = 900.86 | V = 3660.5 (14) Å3 |
Monclinic, C2/c | Z = 4 |
a = 17.514 (4) Å | Mo Kα radiation |
b = 10.639 (2) Å | µ = 3.70 mm−1 |
c = 20.106 (4) Å | T = 0 K |
α = 90° | × × mm |
β = 102.29 (3)° | |
Data collection top
17044 measured reflections | 4277 reflections with I > 2σ(I) |
4363 independent reflections | Rint = 0.022 |
Refinement top
R[F2 > 2σ(F2)] = 0.049 | 0 restraints |
wR(F2) = 0.259 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.18 | (Δ/σ)max = 0.946 |
4363 reflections | Δρmax = 2.01 e Å−3 |
105 parameters | Δρmin = −2.68 e Å−3 |
Special details top
Experimental. Since this work regards a space-group change and the experimental Reflection intensities are nt retained by the original Journal, the calculated Reflection intensities used in this work are obtained following the method reported in: 22 Space-group changes Dore Augusto CLEMENTE and Armando Marzotto Acta Crystallographica Section B (2003) B59, 43–50. |
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is nt relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Re1 | 0.5 | 0.22045 | 0.25 | 0.02* | |
Cl1 | 0.55910 | 0.4008 | 0.20727 | 0.02* | |
S1 | 0.45175 | 0.029 | 0.28915 | 0.02* | 0.5 |
S2 | 0.4803 | −0.23605 | 0.24985 | 0.02* | 0.5 |
P1 | 0.4005 | 0.23975 | 0.14235 | 0.02* | |
N1 | 0.54705 | 0.09350 | 0.2145 | 0.02* | 0.5 |
N3 | 0.54470 | −0.02250 | 0.2096 | 0.02* | 0.5 |
C1 | 0.5 | −0.07550 | 0.25 | 0.02* | |
C2 | 0.39345 | −0.25350 | 0.2865 | 0.02* | 0.5 |
C4 | 0.43975 | 0.25665 | 0.0651 | 0.02* | |
C5 | 0.4151 | 0.34955 | 0.01795 | 0.02* | |
C6 | 0.4473 | 0.35930 | −0.03940 | 0.02* | |
C7 | 0.50405 | 0.2761 | −0.04945 | 0.02* | |
C8 | 0.52865 | 0.1832 | −0.00225 | 0.02* | |
C9 | 0.4965 | 0.17345 | 0.05505 | 0.02* | |
C10 | 0.33485 | 0.1048 | 0.12515 | 0.02* | |
C11 | 0.3175 | 0.0453 | 0.0623 | 0.02* | |
C12 | 0.26285 | −0.05100 | 0.05055 | 0.02* | |
C13 | 0.22545 | −0.08785 | 0.1017 | 0.02* | |
C14 | 0.2428 | −0.02835 | 0.16455 | 0.02* | |
C15 | 0.29745 | 0.068 | 0.17625 | 0.02* | |
C16 | 0.33225 | 0.37235 | 0.13845 | 0.02* | |
C17 | 0.36255 | 0.49205 | 0.15345 | 0.02* | |
C18 | 0.3125 | 0.59355 | 0.15335 | 0.02* | |
C19 | 0.23225 | 0.57525 | 0.1382 | 0.02* | |
C20 | 0.20195 | 0.4555 | 0.1232 | 0.02* | |
C21 | 0.25195 | 0.35405 | 0.1233 | 0.02* | |
Geometric parameters (Å, º) top
Re1—Cl1 | 2.4227 | C6—C7 | 1.3776 |
Re1—S1 | 2.4012 | C7—C8 | 1.3744 |
Re1—P1 | 2.4815 | C8—C9 | 1.3897 |
Re1—N1 | 1.8064 | C10—C11 | 1.388 |
S1—C1 | 1.6891 | C10—C15 | 1.3872 |
S2—C1 | 1.7425 | C11—C12 | 1.3876 |
S2—C2 | 1.8353 | C12—C13 | 1.3882 |
P1—C4 | 1.8363 | C13—C14 | 1.388 |
P1—C10 | 1.8258 | C14—C15 | 1.3879 |
P1—C16 | 1.8399 | C16—C17 | 1.3879 |
N1—N3 | 1.238 | C16—C21 | 1.3879 |
N3—C1 | 1.3643 | C17—C18 | 1.3906 |
C4—C5 | 1.3739 | C18—C19 | 1.387 |
C4—C9 | 1.3776 | C19—C20 | 1.3884 |
C5—C6 | 1.3911 | C20—C21 | 1.3896 |
| | | |
Cl1···C17 | 3.5182 | C9···C11 | 3.4501 |
Cl1···C17i | 3.0053 | C9···S1i | 3.4332 |
Cl1···C14ii | 3.5824 | C11···C9 | 3.4501 |
S1···C15 | 3.1649 | C14···Cl1vii | 3.5824 |
S1···C9i | 3.4332 | C15···S1 | 3.1649 |
S1···C20iii | 3.6032 | C15···C21 | 3.2663 |
S2···C18iv | 3.6415 | C15···N1i | 3.1255 |
N1···C9 | 3.2522 | C15···N3i | 3.3371 |
N1···C15i | 3.1255 | C17···Cl1 | 3.5182 |
N3···C15i | 3.3371 | C17···C5 | 3.411 |
C2···C18iv | 3.1952 | C17···Cl1i | 3.0053 |
C2···C7v | 3.4597 | C18···S2viii | 3.6415 |
C2···C20iii | 3.5105 | C18···C2viii | 3.1952 |
C5···C17 | 3.411 | C20···S1ix | 3.6032 |
C7···C2vi | 3.4597 | C20···C2ix | 3.5105 |
C9···N1 | 3.2522 | C21···C15 | 3.2663 |
| | | |
Cl1—Re1—S1 | 174.15 | S1—C1—N3 | 114.38 |
Cl1—Re1—P1 | 84.2 | S1—C1—S1i | 97.67 |
Cl1—Re1—N1 | 100.76 | S1—C1—S2i | 139.73 |
Cl1—Re1—Cl1i | 75.26 | S1—C1—N3i | 16.88 |
Cl1—Re1—S1i | 110.42 | S2—C1—N3 | 122.86 |
Cl1—Re1—P1i | 88.28 | S1i—C1—S2 | 139.73 |
Cl1—Re1—N1i | 175.97 | S2—C1—S2i | 22.8 |
S1—Re1—P1 | 97.2 | S2—C1—N3i | 105.53 |
S1—Re1—N1 | 73.58 | S1i—C1—N3 | 16.88 |
Cl1i—Re1—S1 | 110.42 | S2i—C1—N3 | 105.53 |
S1—Re1—S1i | 63.95 | N3—C1—N3i | 131.18 |
S1—Re1—P1i | 90.86 | S1i—C1—S2i | 121.84 |
S1—Re1—N1i | 9.68 | S1i—C1—N3i | 114.38 |
P1—Re1—N1 | 90.68 | S2i—C1—N3i | 122.86 |
Cl1i—Re1—P1 | 88.28 | P1—C4—C5 | 122.33 |
S1i—Re1—P1 | 90.86 | P1—C4—C9 | 118.22 |
P1—Re1—P1i | 170.51 | C5—C4—C9 | 119.44 |
P1—Re1—N1i | 96.42 | C4—C5—C6 | 120.15 |
Cl1i—Re1—N1 | 175.97 | C5—C6—C7 | 120.41 |
S1i—Re1—N1 | 9.68 | C6—C7—C8 | 119.39 |
P1i—Re1—N1 | 96.42 | C7—C8—C9 | 120.22 |
N1—Re1—N1i | 83.22 | C4—C9—C8 | 120.39 |
Cl1i—Re1—S1i | 174.15 | P1—C10—C11 | 122.55 |
Cl1i—Re1—P1i | 84.2 | P1—C10—C15 | 117.34 |
Cl1i—Re1—N1i | 100.76 | C11—C10—C15 | 119.95 |
S1i—Re1—P1i | 97.2 | C10—C11—C12 | 120.08 |
S1i—Re1—N1i | 73.58 | C11—C12—C13 | 119.97 |
P1i—Re1—N1i | 90.68 | C12—C13—C14 | 119.95 |
Re1—S1—C1 | 99.19 | C13—C14—C15 | 120.04 |
C1—S2—C2 | 106.21 | C10—C15—C14 | 120.01 |
Re1—P1—C4 | 115.22 | P1—C16—C17 | 118.65 |
Re1—P1—C10 | 113.4 | P1—C16—C21 | 121.37 |
Re1—P1—C16 | 115.46 | C17—C16—C21 | 119.94 |
C4—P1—C10 | 104.53 | C16—C17—C18 | 120.03 |
C4—P1—C16 | 104.22 | C17—C18—C19 | 120.02 |
C10—P1—C16 | 102.57 | C18—C19—C20 | 119.94 |
Re1—N1—N3 | 140.04 | C19—C20—C21 | 120.05 |
N1—N3—C1 | 112.22 | C16—C21—C20 | 120.01 |
S1—C1—S2 | 121.84 | | |
| | | |
P1—Re1—S1—C1 | 87.43 | C16—P1—C4—C5 | −2.57 |
N1—Re1—S1—C1 | −1.16 | Re1—P1—C4—C9 | 49.16 |
Cl1i—Re1—S1—C1 | 178.28 | C10—P1—C4—C5 | 104.74 |
S1i—Re1—S1—C1 | 0 | C16—P1—C10—C11 | 102.6 |
P1i—Re1—S1—C1 | −97.59 | Re1—P1—C16—C17 | 52.29 |
N1i—Re1—S1—C1 | 173.4 | Re1—P1—C10—C11 | −132.21 |
Cl1—Re1—S1i—C1 | 178.28 | C4—P1—C10—C11 | −5.93 |
S1—Re1—S1i—C1 | 0 | C10—P1—C16—C17 | 176.12 |
P1—Re1—S1i—C1 | −97.59 | Re1—P1—C10—C15 | 52.43 |
N1—Re1—S1i—C1 | 173.4 | C10—P1—C4—C9 | −75.97 |
Cl1—Re1—P1—C4 | 48.23 | C16—P1—C4—C9 | 176.71 |
S1—Re1—P1—C4 | −126.05 | C16—P1—C10—C15 | −72.77 |
N1—Re1—P1—C4 | −52.52 | Re1—P1—C16—C21 | −125.41 |
Cl1i—Re1—P1—C4 | 123.59 | C4—P1—C16—C17 | −75.12 |
S1i—Re1—P1—C4 | −62.20 | C4—P1—C16—C21 | 107.18 |
N1i—Re1—P1—C4 | −135.77 | C10—P1—C16—C21 | −1.58 |
Cl1—Re1—P1—C10 | 168.62 | C4—P1—C10—C15 | 178.71 |
S1—Re1—P1—C10 | −5.66 | Re1—N1—N3—C1 | −10.81 |
N1—Re1—P1—C10 | 67.87 | N1—N3—C1—S2 | 175.62 |
Cl1i—Re1—P1—C10 | −116.02 | N1—N3—C1—N3i | 4.35 |
S1i—Re1—P1—C10 | 58.19 | N1—N3—C1—S1 | 6.41 |
N1i—Re1—P1—C10 | −15.38 | N1—N3—C1—S2i | −168.04 |
Cl1—Re1—P1—C16 | −73.43 | N1—N3—C1—S1i | −2.11 |
S1—Re1—P1—C16 | 112.29 | C9—C4—C5—C6 | −0.02 |
N1—Re1—P1—C16 | −174.18 | P1—C4—C5—C6 | 179.26 |
Cl1i—Re1—P1—C16 | 1.92 | C5—C4—C9—C8 | 0.02 |
S1i—Re1—P1—C16 | 176.14 | P1—C4—C9—C8 | −179.30 |
N1i—Re1—P1—C16 | 102.57 | C4—C5—C6—C7 | 0.03 |
Cl1—Re1—N1—N3 | −174.10 | C5—C6—C7—C8 | −0.02 |
S1—Re1—N1—N3 | 7.43 | C6—C7—C8—C9 | 0 |
P1—Re1—N1—N3 | −89.88 | C7—C8—C9—C4 | 0 |
S1i—Re1—N1—N3 | 1.24 | P1—C10—C11—C12 | −175.30 |
P1i—Re1—N1—N3 | 96.43 | C11—C10—C15—C14 | 0.08 |
N1i—Re1—N1—N3 | 6.5 | C15—C10—C11—C12 | −0.06 |
Re1—S1—C1—S1i | 0 | P1—C10—C15—C14 | 175.57 |
Re1—S1—C1—S2 | −171.82 | C10—C11—C12—C13 | 0.03 |
Re1—S1—C1—N3 | −2.49 | C11—C12—C13—C14 | −0.03 |
Re1—S1i—C1—S1 | 0 | C12—C13—C14—C15 | 0.05 |
Re1—S1—C1—S2i | 169.22 | C13—C14—C15—C10 | −0.08 |
Re1—S1—C1—N3i | 172.18 | P1—C16—C17—C18 | −177.68 |
Re1—S1i—C1—S2 | 169.22 | C21—C16—C17—C18 | 0.05 |
Re1—S1i—C1—N3 | 172.18 | P1—C16—C21—C20 | 177.63 |
C2—S2—C1—N3 | −160.23 | C17—C16—C21—C20 | −0.04 |
C2—S2—C1—S1 | 8.2 | C16—C17—C18—C19 | −0.06 |
C2—S2—C1—S2i | 155.37 | C17—C18—C19—C20 | 0.06 |
C2—S2—C1—S1i | −159.20 | C18—C19—C20—C21 | −0.06 |
C2—S2—C1—N3i | 12.96 | C19—C20—C21—C16 | 0.05 |
Re1—P1—C4—C5 | −130.13 | | |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) x+1/2, y+1/2, z; (iii) −x+1/2, y−1/2, −z+1/2; (iv) x, y−1, z; (v) x, −y, z+1/2; (vi) x, −y, z−1/2; (vii) x−1/2, y−1/2, z; (viii) x, y+1, z; (ix) −x+1/2, y+1/2, −z+1/2. |
(25) bis(eta$6!-Benzene)-chromium hydroxide trihydrate
top
Crystal data top
(C12H12Cr+)·(OH−)·3(H2O) | Z = 4 |
Mr = 279.28 | F(000) = 560 |
Orthorhombic, Cmca | Dx = 1.340 Mg m−3 |
Hall symbol: -C 2bc 2 | Mo K\a radiation, λ = 0.71070 Å |
a = 16.409 (3) Å | µ = 0.85 mm−1 |
b = 10.506 (4) Å | T = 0 K |
c = 7.825 (3) Å | × × mm |
V = 1349.0 (8) Å3 | |
Crystal data top
(C12H12Cr+)·(OH−)·3(H2O) | V = 1349.0 (8) Å3 |
Mr = 279.28 | Z = 4 |
Orthorhombic, Cmca | Mo K\a radiation |
a = 16.409 (3) Å | µ = 0.85 mm−1 |
b = 10.506 (4) Å | T = 0 K |
c = 7.825 (3) Å | × × mm |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cr1 | 0 | 0 | 0 | 0.02* | |
C1 | 0.0429 | 0.0134 | 0.25795 | 0.02* | |
C3 | 0.0849 | 0.10055 | 0.15615 | 0.02* | |
C4 | 0.043 | 0.18765 | 0.05095 | 0.02* | |
O1 | 0.22135 | 0.3721 | 0.07305 | 0.02* | |
H1 | 0.07141 | −0.04432 | 0.32537 | 0.026* | |
H3 | 0.14157 | 0.10118 | 0.15774 | 0.026* | |
H4 | 0.07169 | 0.24441 | −0.01760 | 0.026* | |
Geometric parameters (Å, º) top
Cr1—C1 | 2.1423 | C3—C4 | 1.4099 |
Cr1—C3 | 2.133 | C4—C4i | 1.4112 |
Cr1—C4 | 2.1315 | C1—H1 | 0.93 |
C1—C3 | 1.3956 | C3—H3 | 0.93 |
C1—C1i | 1.4079 | C4—H4 | 0.93 |
| | | |
Cr1···H3i | 2.8372 | C3···H4vi | 3.036 |
O1···O1ii | 2.9245 | C4···H1v | 3.0139 |
O1···O1iii | 2.9205 | H1···O1vii | 2.7306 |
O1···O1iv | 2.962 | H1···C4vii | 3.0139 |
O1···H1v | 2.7306 | H3···O1iv | 2.8982 |
O1···H4 | 2.8869 | H4···C3viii | 3.036 |
O1···H3iv | 2.8982 | H4···O1 | 2.8869 |
| | | |
C1—Cr1—C3 | 38.11 | C1i—Cr1—C3ix | 141.89 |
C1—Cr1—C4 | 69.77 | C3ix—Cr1—C3i | 180 |
C1—Cr1—C1ix | 141.63 | C3ix—Cr1—C4i | 141.39 |
C1—Cr1—C3ix | 110.96 | C1x—Cr1—C4ix | 82.63 |
C1—Cr1—C4ix | 97.37 | C3x—Cr1—C4ix | 69.57 |
C1—Cr1—C1x | 180 | C4ix—Cr1—C4x | 38.66 |
C1—Cr1—C3x | 141.89 | C1i—Cr1—C4ix | 110.23 |
C1—Cr1—C4x | 110.23 | C3i—Cr1—C4ix | 141.39 |
C1—Cr1—C1i | 38.37 | C4ix—Cr1—C4i | 180 |
C1—Cr1—C3i | 69.04 | C1x—Cr1—C3x | 38.11 |
C1—Cr1—C4i | 82.63 | C1x—Cr1—C4x | 69.77 |
C3—Cr1—C4 | 38.61 | C1x—Cr1—C1i | 141.63 |
C1ix—Cr1—C3 | 110.96 | C1x—Cr1—C3i | 110.96 |
C3—Cr1—C3ix | 98.44 | C1x—Cr1—C4i | 97.37 |
C3—Cr1—C4ix | 110.43 | C3x—Cr1—C4x | 38.61 |
C1x—Cr1—C3 | 141.89 | C1i—Cr1—C3x | 110.96 |
C3—Cr1—C3x | 180 | C3x—Cr1—C3i | 98.44 |
C3—Cr1—C4x | 141.39 | C3x—Cr1—C4i | 110.43 |
C1i—Cr1—C3 | 69.04 | C1i—Cr1—C4x | 97.37 |
C3—Cr1—C3i | 81.56 | C3i—Cr1—C4x | 110.43 |
C3—Cr1—C4i | 69.57 | C4x—Cr1—C4i | 141.34 |
C1ix—Cr1—C4 | 97.37 | C1i—Cr1—C3i | 38.11 |
C3ix—Cr1—C4 | 110.43 | C1i—Cr1—C4i | 69.77 |
C4—Cr1—C4ix | 141.34 | C3i—Cr1—C4i | 38.61 |
C1x—Cr1—C4 | 110.23 | Cr1—C1—C3 | 70.59 |
C3x—Cr1—C4 | 141.39 | Cr1—C1—C1i | 70.82 |
C4—Cr1—C4x | 180 | C1i—C1—C3 | 119.59 |
C1i—Cr1—C4 | 82.63 | Cr1—C3—C1 | 71.31 |
C3i—Cr1—C4 | 69.57 | Cr1—C3—C4 | 70.64 |
C4—Cr1—C4i | 38.66 | C1—C3—C4 | 121.21 |
C1ix—Cr1—C3ix | 38.11 | Cr1—C4—C3 | 70.75 |
C1ix—Cr1—C4ix | 69.77 | Cr1—C4—C4i | 70.67 |
C1ix—Cr1—C1x | 38.37 | C3—C4—C4i | 119.19 |
C1ix—Cr1—C3x | 69.04 | Cr1—C1—H1 | 131.07 |
C1ix—Cr1—C4x | 82.63 | C3—C1—H1 | 120.2 |
C1ix—Cr1—C1i | 180 | C1i—C1—H1 | 120.2 |
C1ix—Cr1—C3i | 141.89 | Cr1—C3—H3 | 131.62 |
C1ix—Cr1—C4i | 110.23 | C1—C3—H3 | 119.39 |
C3ix—Cr1—C4ix | 38.61 | C4—C3—H3 | 119.39 |
C1x—Cr1—C3ix | 69.04 | Cr1—C4—H4 | 130.74 |
C3ix—Cr1—C3x | 81.56 | C3—C4—H4 | 120.41 |
C3ix—Cr1—C4x | 69.57 | C4i—C4—H4 | 120.41 |
| | | |
C4—Cr1—C1—C3 | −28.41 | C1—Cr1—C3—C4 | −134.33 |
C1ix—Cr1—C1—C3 | 47.39 | C1ix—Cr1—C3—C4 | 74.96 |
C3ix—Cr1—C1—C3 | 76.49 | C3ix—Cr1—C3—C4 | 112.3 |
C4ix—Cr1—C1—C3 | 113.92 | C4ix—Cr1—C3—C4 | 150.33 |
C3x—Cr1—C1—C3 | 179.98 | C1x—Cr1—C3—C4 | 45.67 |
C4x—Cr1—C1—C3 | 151.59 | C4x—Cr1—C3—C4 | 180 |
C1i—Cr1—C1—C3 | −132.61 | C1i—Cr1—C3—C4 | −105.04 |
C3i—Cr1—C1—C3 | −103.51 | C3i—Cr1—C3—C4 | −67.70 |
C4i—Cr1—C1—C3 | −66.08 | C4i—Cr1—C3—C4 | −29.67 |
C3—Cr1—C1—C1i | 132.61 | C1x—Cr1—C4—C3 | −151.94 |
C4—Cr1—C1—C1i | 104.2 | C1ix—Cr1—C4—C3 | −114.58 |
C3x—Cr1—C4—C3 | 180 | C3ix—Cr1—C4—C3 | −77.57 |
C1i—Cr1—C4—C3 | 65.42 | C1—Cr1—C4—C3 | 28.06 |
C3i—Cr1—C4—C3 | 102.43 | C3—Cr1—C4—C4i | −132.06 |
C4i—Cr1—C4—C3 | 132.06 | C4ix—Cr1—C4—C3 | −47.94 |
C1—Cr1—C4—C4i | −104.00 | C1i—C1—C3—C4 | −0.97 |
C4—Cr1—C3—C1 | 134.33 | C3—C1—C1i—C3i | 0 |
C1ix—Cr1—C3—C1 | −150.71 | Cr1—C1—C3—C4 | 52.1 |
C3ix—Cr1—C3—C1 | −113.37 | C3—C1—C1i—Cr1 | 52.97 |
C4ix—Cr1—C3—C1 | −75.34 | C1i—C1—C3—Cr1 | −53.07 |
C1x—Cr1—C3—C1 | 179.98 | C1—C3—C4—Cr1 | −52.40 |
C4x—Cr1—C3—C1 | −45.67 | C1—C3—C4—C4i | 0.97 |
C1i—Cr1—C3—C1 | 29.29 | Cr1—C3—C4—C4i | 53.37 |
C3i—Cr1—C3—C1 | 66.63 | C3—C4—C4i—Cr1 | −53.41 |
C4i—Cr1—C3—C1 | 104.66 | C3—C4—C4i—C3i | 0 |
Symmetry codes: (i) −x, y, z; (ii) −x+1/2, y, −z+1/2; (iii) x, −y+1, −z; (iv) −x+1/2, −y+1/2, −z; (v) x, y+1/2, −z+1/2; (vi) x, −y+1/2, z+1/2; (vii) x, y−1/2, −z+1/2; (viii) x, −y+1/2, z−1/2; (ix) x, −y, −z; (x) −x, −y, −z. |
(26)
mer,
trans-Trichloro-phenylimido-bis(trimethylphosphine)-rhenium
top
Crystal data top
C12H23Cl3NP2Re | Z = 4 |
Mr = 535.80 | F(000) = 940 |
Orthorhombic, Cmcm | Dx = 1.692 Mg m−3 |
Hall symbol: -C 2c 2 | Mo K\a radiation, λ = 0.71073 Å |
a = 11.0341 (10) Å | µ = 6.58 mm−1 |
b = 16.814 (2) Å | T = 0 K |
c = 10.844 (1) Å | × × mm |
V = 2011.9 (4) Å3 | |
Crystal data top
C12H23Cl3NP2Re | V = 2011.9 (4) Å3 |
Mr = 535.80 | Z = 4 |
Orthorhombic, Cmcm | Mo K\a radiation |
a = 11.0341 (10) Å | µ = 6.58 mm−1 |
b = 16.814 (2) Å | T = 0 K |
c = 10.844 (1) Å | × × mm |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Re1 | 0.5 | 0.3032 | 0.25 | 0.02* | |
Cl1 | 0.28155 | 0.31015 | 0.25 | 0.02* | |
Cl3 | 0.5 | 0.4478 | 0.25 | 0.02* | |
P1 | 0.5 | 0.3209 | 0.02735 | 0.02* | |
N1 | 0.5 | 0.2024 | 0.25 | 0.02* | |
C1 | 0.5 | 0.11915 | 0.25 | 0.02* | |
C2 | 0.39255 | 0.0779 | 0.25 | 0.02* | |
C3 | 0.3911 | 0.00005 | 0.25 | 0.02* | |
C4 | 0.5 | −0.04080 | 0.25 | 0.02* | |
C7 | 0.5 | 0.2267 | −0.05155 | 0.02* | |
C8 | 0.62874 | 0.37418 | −0.03657 | 0.02* | |
Geometric parameters (Å, º) top
Re1—Cl1 | 2.4132 (3) | P1—C8 | 1.8168 |
Re1—Cl3 | 2.4313 (3) | N1—C1 | 1.3998 (2) |
Re1—P1 | 2.4327 (3) | C1—C2 | 1.3736 (2) |
Re1—N1 | 1.6949 (2) | C1—C2i | 1.3736 (2) |
Re1—Cl1i | 2.4132 (3) | C2—C3 | 1.3091 (2) |
Re1—P1i | 2.4327 (3) | C3—C4 | 1.3841 (2) |
P1—C7 | 1.8002 (2) | | |
| | | |
Cl1—Re1—Cl3 | 87.22 | Cl1i—Re1—P1i | 89.66 |
Cl1—Re1—P1 | 89.66 | Re1—P1—C7 | 111.35 |
Cl1—Re1—N1 | 92.78 | Re1—P1—C8 | 116.04 |
Cl1—Re1—Cl1i | 174.45 | Re1—P1—C8ii | 116.04 |
Cl1—Re1—P1i | 89.66 | C7—P1—C8 | 104.63 |
Cl3—Re1—P1 | 82.97 | C7—P1—C8ii | 104.63 |
Cl3—Re1—N1 | 180 | C8—P1—C8ii | 102.86 |
Cl1i—Re1—Cl3 | 87.22 | Re1—N1—C1 | 180 |
Cl3—Re1—P1i | 82.97 | N1—C1—C2 | 120.33 |
P1—Re1—N1 | 97.03 | N1—C1—C2i | 120.33 |
Cl1i—Re1—P1 | 89.66 | C2—C1—C2i | 119.35 |
P1—Re1—P1i | 165.95 | C1—C2—C3 | 121.03 |
Cl1i—Re1—N1 | 92.78 | C2—C3—C4 | 119.05 |
P1i—Re1—N1 | 97.03 | C3—C4—C3i | 120.49 |
| | | |
Cl1—Re1—P1—C7 | −92.75 | Cl3—Re1—P1—C8 | 60.48 |
Cl3—Re1—P1—C7 | 180 | N1—Re1—P1—C8 | −119.52 |
N1—Re1—P1—C7 | 0 | N1—C1—C2—C3 | 180 |
Cl1—Re1—P1—C8 | 147.73 | C1—C2—C3—C4 | 0 |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+1, y, z. |
(27) mu!3$-eta$4!,eta$4!-Buta-1,3-dien-1,4-diyl)-(mu!2$-hydrido)-tris (eta$4!-
cyclo-octa-1,5-diene)-tri-iridium
top
Crystal data top
C12H13Ir3 | Z = 4 |
Mr = 733.88 | F(000) = 1212 |
Orthorhombic, Cmcm | Dx = 1.684 Mg m−3 |
Hall symbol: -C 2c 2 | Mo K\a radiation, λ = 0.71073 Å |
a = 11.2624 Å | µ = 13.99 mm−1 |
b = 9.711 Å | T = 0 K |
c = 25.998 Å | × × mm |
V = 2843.38 Å3 | |
Crystal data top
C12H13Ir3 | V = 2843.38 Å3 |
Mr = 733.88 | Z = 4 |
Orthorhombic, Cmcm | Mo K\a radiation |
a = 11.2624 Å | µ = 13.99 mm−1 |
b = 9.711 Å | T = 0 K |
c = 25.998 Å | × × mm |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ir1 | 0 | 0.2933 | 0.25 | 0.02* | |
Ir2 | 0 | 0.0937 | 0.3243 | 0.02* | |
C1 | −0.06657 | −0.00873 | 0.25 | 0.02* | |
C2 | −0.11713 | 0.12718 | 0.25 | 0.02* | |
C5 | 0.12583 | 0.44973 | 0.22328 | 0.02* | |
C6 | 0.0718 | 0.55247 | 0.18465 | 0.02* | |
Geometric parameters (Å, º) top
Ir1—C2 | 2.0839 | Ir2—C2i | 2.3616 |
Ir1—C5 | 2.1905 | C1—C2 | 1.4374 |
Ir1—C2i | 2.0839 | C1—C1i | 1.4995 |
Ir2—C1 | 2.2984 | C5—C6 | 1.5409 |
Ir2—C2 | 2.3616 | C5—C5ii | 1.3893 |
Ir2—C1i | 2.2984 | C6—C6iii | 1.6173 |
| | | |
C1···C5iv | 3.5562 | C5···C1vi | 3.5562 |
C1···C5v | 3.5562 | C5···C2vi | 3.4398 |
C2···C5iv | 3.4398 | C5···C1vii | 3.5562 |
C2···C5v | 3.4398 | C5···C2vii | 3.4398 |
| | | |
C2—Ir1—C5 | 161.15 | C2—Ir2—C2i | 67.92 |
C2—Ir1—C2i | 78.55 | C1i—Ir2—C2i | 35.9 |
C2—Ir1—C5i | 97.31 | Ir2—C1—C2 | 74.45 |
C2—Ir1—C5ii | 161.15 | Ir2—C1—Ir2i | 114.37 |
C2—Ir1—C5iii | 97.31 | Ir2—C1—C1i | 70.96 |
C2i—Ir1—C5 | 97.31 | Ir2i—C1—C2 | 74.45 |
C5—Ir1—C5i | 92.19 | C1i—C1—C2 | 113.34 |
C5—Ir1—C5ii | 36.98 | Ir2i—C1—C1i | 70.96 |
C5—Ir1—C5iii | 80.62 | Ir1—C2—Ir2 | 75.7 |
C2i—Ir1—C5i | 161.15 | Ir1—C2—C1 | 117.39 |
C2i—Ir1—C5ii | 97.31 | Ir1—C2—Ir2i | 75.7 |
C2i—Ir1—C5iii | 161.15 | Ir2—C2—C1 | 69.65 |
C5i—Ir1—C5ii | 80.62 | Ir2—C2—Ir2i | 109.76 |
C5i—Ir1—C5iii | 36.98 | Ir2i—C2—C1 | 69.65 |
C5ii—Ir1—C5iii | 92.19 | Ir1—C5—C6 | 113.59 |
C1—Ir2—C2 | 35.9 | Ir1—C5—C5ii | 71.51 |
C1—Ir2—C1i | 38.08 | C5ii—C5—C6 | 130.68 |
C1—Ir2—C2i | 63.54 | C5—C6—C6iii | 113.26 |
C1i—Ir2—C2 | 63.54 | | |
| | | |
C5i—Ir1—C5—C6 | −55.92 | Ir1—C5—C6—C6iii | 17.04 |
C5ii—Ir1—C5—C6 | −127.15 | C5ii—C5—C6—C6iii | −68.32 |
C2i—Ir1—C5—C6 | 140.39 | C6—C5—C5ii—Ir1 | 105.61 |
C5iii—Ir1—C5—C6 | −20.67 | C6—C5—C5ii—C6ii | 0 |
C1—Ir2—C2—Ir1 | −126.93 | C5—C6—C6iii—C5iii | 0 |
Ir2—C1—C2—Ir1 | 60.73 | | |
Symmetry codes: (i) −x, y, −z+1/2; (ii) x, y, −z+1/2; (iii) −x, y, z; (iv) x−1/2, y−1/2, z; (v) x−1/2, y−1/2, −z+1/2; (vi) x+1/2, y+1/2, z; (vii) x+1/2, y+1/2, −z+1/2. |
(28) bis(1,4-Dimethyl-9-triptycyl)ethyne chloroform solvate
top
Crystal data top
C46H34·2(CHCl3) | γ = 90° |
Mr = 825.47 | V = 2040.4 (6) Å3 |
Monclinic, P21/n | Z = 2 |
Hall symbol: -P 2yn | F(000) = 780 |
a = 15.592 (2) Å | Dx = 1.285 Mg m−3 |
b = 8.642 (2) Å | Mo K\a radiation, λ = 0.71070 Å |
c = 16.677 (2) Å | µ = 0.45 mm−1 |
α = 90° | T = 0 K |
β = 114.773 (9)° | × × mm |
Crystal data top
C46H34·2(CHCl3) | γ = 90° |
Mr = 825.47 | V = 2040.4 (6) Å3 |
Monclinic, P21/n | Z = 2 |
a = 15.592 (2) Å | Mo K\a radiation |
b = 8.642 (2) Å | µ = 0.45 mm−1 |
c = 16.677 (2) Å | T = 0 K |
α = 90° | × × mm |
β = 114.773 (9)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
C1 | 0.0058 | 1.142 | 0.20020 | 0.02* | |
C3 | 0.00925 | 1.19650 | 0.2804 | 0.02* | |
C5 | 0.0084 | 1.1005 | 0.3457 | 0.02* | |
C7 | 0.0039 | 0.9415 | 0.33505 | 0.02* | |
C8 | 0.0018 | 0.8845 | 0.2561 | 0.02* | |
C11 | 0.15890 | 0.583 | 0.25655 | 0.02* | |
C13 | 0.23125 | 0.5735 | 0.2293 | 0.02* | |
C15 | 0.2303 | 0.6635 | 0.161 | 0.02* | |
C17 | 0.157 | 0.767 | 0.11865 | 0.02* | |
C18 | 0.085 | 0.77750 | 0.14615 | 0.02* | |
C21 | −0.00055 | 0.889 | 0.1086 | 0.02* | |
C22 | 0.00165 | 0.9825 | 0.18915 | 0.02* | |
C25 | −0.00005 | 0.7125 | 0.2345 | 0.02* | |
C26 | 0.08555 | 0.68550 | 0.21425 | 0.02* | |
C29 | −0.08670 | 0.6875 | 0.1487 | 0.02* | |
C31 | −0.08775 | 0.782 | 0.08055 | 0.02* | |
C33 | −0.16145 | 0.773 | −0.00230 | 0.02* | |
C35 | −0.23420 | 0.6675 | −0.01735 | 0.02* | |
C37 | −0.23295 | 0.575 | 0.05025 | 0.02* | |
C39 | −0.15900 | 0.5845 | 0.1341 | 0.02* | |
C41 | 0.00480 | 1.2595 | 0.1336 | 0.02* | |
C43 | 0.0013 | 0.8375 | 0.4064 | 0.02* | |
C45 | −0.00060 | 0.975 | 0.03295 | 0.02* | |
Cl1 | 0.2107 | 0.3817 | 0.5223 | 0.02* | 0.5 |
Cl2 | 0.16785 | 0.40005 | 0.49865 | 0.02* | 0.5 |
Cl4 | 0.11555 | 0.5714 | 0.59945 | 0.02* | 0.5 |
Cl5 | 0.1215 | 0.59745 | 0.61725 | 0.02* | 0.5 |
Cl7 | 0.25745 | 0.3362 | 0.68585 | 0.02* | 0.5 |
Cl8 | 0.2665 | 0.38545 | 0.68825 | 0.02* | 0.5 |
C47 | 0.2133 | 0.48575 | 0.59875 | 0.02* | 0.5 |
C48 | 0.221 | 0.49565 | 0.60495 | 0.02* | 0.5 |
Geometric parameters (Å, º) top
Cl1—C48 | 1.6462 | C8—C22 | 1.4006 |
Cl1—C47 | 1.5467 | C8—C25 | 1.5269 |
Cl1—Cl2 | 0.6374 | C11—C26 | 1.3835 |
Cl2—C47 | 1.687 | C11—C13 | 1.384 |
Cl2—C48 | 1.8113 | C13—C15 | 1.3742 |
Cl4—Cl5 | 0.3526 | C15—C17 | 1.3887 |
Cl4—C47 | 1.6988 | C17—C18 | 1.3821 |
Cl4—C48 | 1.7361 | C18—C21 | 1.5492 |
Cl5—C47 | 1.8563 | C18—C26 | 1.3834 |
Cl5—C48 | 1.868 | C21—C22 | 1.5556 |
Cl7—C48 | 1.8438 | C21—C31 | 1.5458 |
Cl7—Cl8 | 0.4449 | C21—C45 | 1.464 |
Cl7—C47 | 1.8483 | C25—C26 | 1.5256 |
Cl8—C47 | 1.6216 | C25—C29 | 1.5164 |
Cl8—C48 | 1.5856 | C29—C31 | 1.394 |
C1—C41 | 1.5002 | C29—C39 | 1.3756 |
C1—C3 | 1.3976 | C31—C33 | 1.3802 |
C1—C22 | 1.3886 | C33—C35 | 1.3937 |
C3—C5 | 1.3735 | C35—C37 | 1.3755 |
C5—C7 | 1.3835 | C37—C39 | 1.393 |
C7—C43 | 1.5052 | C45—C45i | 1.1883 |
C7—C8 | 1.3933 | C47—C48 | 0.1484 |
| | | |
Cl5···C3ii | 3.6272 | C13···C17v | 3.5748 |
Cl5···C5ii | 3.5138 | C17···C45i | 3.4847 |
Cl7···C3iii | 3.5766 | C17···C13vi | 3.5748 |
Cl8···C3iii | 3.5092 | C33···C45i | 3.5314 |
Cl8···C5iii | 3.5827 | C41···C45 | 2.9582 |
C3···Cl5ii | 3.6272 | C41···C45i | 3.4167 |
C3···Cl7iv | 3.5766 | C45···C33i | 3.5314 |
C3···Cl8iv | 3.5092 | C45···C41i | 3.4167 |
C5···Cl8iv | 3.5827 | C45···C41 | 2.9582 |
C5···Cl5ii | 3.5138 | C45···C17i | 3.4847 |
| | | |
C47—Cl1—C48 | 3.96 | C25—C29—C39 | 126.82 |
Cl2—Cl1—C48 | 94.5 | C31—C29—C39 | 120.4 |
Cl2—Cl1—C47 | 91.38 | C21—C31—C29 | 113.29 |
Cl1—Cl2—C48 | 64.96 | C21—C31—C33 | 126.47 |
Cl1—Cl2—C47 | 66.43 | C29—C31—C33 | 120.24 |
C47—Cl2—C48 | 2.66 | C31—C33—C35 | 119.38 |
Cl5—Cl4—C48 | 106.68 | C33—C35—C37 | 120.11 |
Cl5—Cl4—C47 | 111.33 | C35—C37—C39 | 120.67 |
C47—Cl4—C48 | 4.79 | C29—C39—C37 | 119.21 |
Cl4—Cl5—C48 | 62.9 | C21—C45—C45i | 170.78 |
C47—Cl5—C48 | 4.55 | Cl1—C47—Cl2 | 22.19 |
Cl4—Cl5—C47 | 58.48 | Cl1—C47—Cl4 | 123.04 |
C47—Cl7—C48 | 4.6 | Cl1—C47—Cl5 | 133.13 |
Cl8—Cl7—C47 | 53.23 | Cl1—C47—Cl7 | 96.53 |
Cl8—Cl7—C48 | 48.68 | Cl1—C47—Cl8 | 105.94 |
C47—Cl8—C48 | 5.15 | Cl1—C47—C48 | 130.06 |
Cl7—Cl8—C48 | 119.15 | Cl2—C47—Cl4 | 101.07 |
Cl7—Cl8—C47 | 114.07 | Cl2—C47—Cl5 | 111.06 |
C22—C1—C41 | 126.03 | Cl2—C47—Cl7 | 109.54 |
C3—C1—C41 | 117.69 | Cl2—C47—Cl8 | 121.12 |
C3—C1—C22 | 116.26 | Cl2—C47—C48 | 145.52 |
C1—C3—C5 | 123.09 | Cl4—C47—Cl5 | 10.19 |
C3—C5—C7 | 120.99 | Cl4—C47—Cl7 | 109.82 |
C5—C7—C8 | 116.89 | Cl4—C47—Cl8 | 109.93 |
C5—C7—C43 | 120.55 | Cl4—C47—C48 | 102.14 |
C8—C7—C43 | 122.56 | Cl5—C47—Cl7 | 106.99 |
C7—C8—C25 | 123.9 | Cl5—C47—Cl8 | 104.93 |
C7—C8—C22 | 122.08 | Cl5—C47—C48 | 92.26 |
C22—C8—C25 | 114.02 | Cl7—C47—Cl8 | 12.7 |
C13—C11—C26 | 118.94 | Cl7—C47—C48 | 85.95 |
C11—C13—C15 | 120.76 | Cl8—C47—C48 | 73.4 |
C13—C15—C17 | 120.45 | Cl1—C48—Cl2 | 20.54 |
C15—C17—C18 | 118.9 | Cl1—C48—Cl4 | 115.05 |
C17—C18—C26 | 120.54 | Cl1—C48—Cl5 | 125.42 |
C21—C18—C26 | 113.42 | Cl1—C48—Cl7 | 93.3 |
C17—C18—C21 | 126.03 | Cl1—C48—Cl8 | 103.01 |
C18—C21—C45 | 110.71 | Cl1—C48—C47 | 45.98 |
C18—C21—C22 | 105.68 | Cl2—C48—Cl4 | 94.91 |
C18—C21—C31 | 104.44 | Cl2—C48—Cl5 | 105.18 |
C31—C21—C45 | 111.11 | Cl2—C48—Cl7 | 104.45 |
C22—C21—C31 | 105.69 | Cl2—C48—Cl8 | 115.9 |
C22—C21—C45 | 118.19 | Cl2—C48—C47 | 31.82 |
C1—C22—C8 | 120.67 | Cl4—C48—Cl5 | 10.42 |
C1—C22—C21 | 127.82 | Cl4—C48—Cl7 | 108.37 |
C8—C22—C21 | 111.49 | Cl4—C48—Cl8 | 109.81 |
C8—C25—C26 | 105.62 | Cl4—C48—C47 | 73.07 |
C26—C25—C29 | 106.59 | Cl5—C48—Cl7 | 106.69 |
C8—C25—C29 | 106.42 | Cl5—C48—Cl8 | 105.9 |
C18—C26—C25 | 112.88 | Cl5—C48—C47 | 83.19 |
C11—C26—C18 | 120.4 | Cl7—C48—Cl8 | 12.16 |
C11—C26—C25 | 126.73 | Cl7—C48—C47 | 89.44 |
C25—C29—C31 | 112.79 | Cl8—C48—C47 | 101.45 |
| | | |
Cl2—Cl1—C47—Cl5 | 6.93 | Cl7—Cl8—C48—C47 | 9.39 |
C48—Cl1—C47—Cl5 | 149.12 | C47—Cl8—C48—Cl1 | −47.09 |
Cl2—Cl1—C47—Cl7 | 127.61 | Cl7—Cl8—C48—Cl2 | −20.68 |
C48—Cl1—C47—Cl7 | −90.20 | C47—Cl8—C48—Cl4 | 75.95 |
Cl2—Cl1—C47—Cl8 | 136.32 | Cl7—Cl8—C48—Cl5 | 95.48 |
C48—Cl1—C47—Cl8 | −81.49 | C47—Cl8—C48—Cl5 | 86.09 |
C47—Cl1—Cl2—C48 | 2.43 | C47—Cl8—C48—Cl7 | −9.39 |
C48—Cl1—Cl2—C47 | −2.43 | Cl7—Cl8—C48—Cl1 | −37.69 |
Cl2—Cl1—C48—Cl4 | 11.91 | Cl7—Cl8—C48—Cl4 | 85.34 |
C47—Cl1—C48—Cl4 | −26.03 | Cl7—Cl8—C47—Cl1 | −43.19 |
Cl2—Cl1—C48—Cl5 | 10.76 | C47—Cl8—C48—Cl2 | −30.07 |
C47—Cl1—C48—Cl5 | −27.18 | Cl7—Cl8—C47—C48 | −171.02 |
C48—Cl1—C47—Cl2 | 142.19 | C48—Cl8—C47—Cl1 | 127.83 |
Cl2—Cl1—C47—Cl4 | 8.82 | C41—C1—C22—C8 | −179.11 |
C48—Cl1—C47—Cl4 | 151.01 | C3—C1—C22—C21 | −178.53 |
Cl2—Cl1—C48—Cl8 | 131.38 | C41—C1—C3—C5 | 178.53 |
C47—Cl1—C48—Cl8 | 93.44 | C3—C1—C22—C8 | −0.50 |
Cl2—Cl1—C48—C47 | 37.94 | C22—C1—C3—C5 | −0.19 |
Cl2—Cl1—C47—C48 | −142.19 | C41—C1—C22—C21 | 2.86 |
C47—Cl1—C48—Cl7 | 86.03 | C1—C3—C5—C7 | −0.06 |
C47—Cl1—C48—Cl2 | −37.94 | C3—C5—C7—C43 | −178.93 |
Cl2—Cl1—C48—Cl7 | 123.96 | C3—C5—C7—C8 | 0.97 |
C47—Cl2—C48—Cl1 | 123.02 | C43—C7—C8—C25 | −2.08 |
C47—Cl2—C48—Cl4 | −46.16 | C43—C7—C8—C22 | 178.22 |
C48—Cl2—C47—Cl4 | 131.55 | C5—C7—C8—C22 | −1.68 |
Cl1—Cl2—C48—Cl4 | −169.18 | C5—C7—C8—C25 | 178.02 |
C48—Cl2—C47—Cl5 | 129.44 | C22—C8—C25—C29 | −56.44 |
Cl1—Cl2—C47—Cl7 | −56.62 | C7—C8—C22—C1 | 1.48 |
Cl1—Cl2—C47—Cl5 | −174.58 | C25—C8—C22—C1 | −178.24 |
C48—Cl2—C47—Cl1 | −55.98 | C25—C8—C22—C21 | 0.08 |
Cl1—Cl2—C47—C48 | 55.98 | C7—C8—C22—C21 | 179.81 |
Cl1—Cl2—C47—Cl4 | −172.47 | C22—C8—C25—C26 | 56.6 |
C47—Cl2—C48—Cl7 | 64.25 | C7—C8—C25—C29 | 123.84 |
Cl1—Cl2—C48—Cl8 | −54.36 | C7—C8—C25—C26 | −123.12 |
C47—Cl2—C48—Cl8 | 68.66 | C13—C11—C26—C25 | 179.95 |
Cl1—Cl2—C48—C47 | −123.02 | C13—C11—C26—C18 | −0.36 |
Cl1—Cl2—C48—Cl5 | −170.93 | C26—C11—C13—C15 | −0.39 |
C47—Cl2—C48—Cl5 | −47.91 | C11—C13—C15—C17 | 0.68 |
C48—Cl2—C47—Cl8 | −106.85 | C13—C15—C17—C18 | −0.22 |
Cl1—Cl2—C48—Cl7 | −58.77 | C15—C17—C18—C26 | −0.53 |
C48—Cl2—C47—Cl7 | −112.60 | C15—C17—C18—C21 | 178.21 |
Cl1—Cl2—C47—Cl8 | −50.87 | C21—C18—C26—C25 | 1.67 |
C48—Cl4—C47—Cl5 | 14.48 | C17—C18—C21—C22 | −123.93 |
C47—Cl4—C48—Cl8 | −96.37 | C17—C18—C21—C45 | 5.17 |
Cl5—Cl4—C48—C47 | 165.93 | C26—C18—C21—C22 | 54.89 |
C47—Cl4—C48—Cl7 | −83.58 | C17—C18—C21—C31 | 124.83 |
Cl5—Cl4—C48—Cl8 | 69.56 | C21—C18—C26—C11 | −178.06 |
Cl5—Cl4—C47—Cl1 | −172.18 | C17—C18—C26—C11 | 0.82 |
C48—Cl4—C47—Cl1 | −157.70 | C17—C18—C26—C25 | −179.45 |
Cl5—Cl4—C47—Cl2 | −168.80 | C26—C18—C21—C31 | −56.35 |
C48—Cl4—C47—Cl2 | −154.32 | C26—C18—C21—C45 | −176.02 |
Cl5—Cl4—C48—Cl1 | −174.81 | C18—C21—C31—C29 | 55.29 |
Cl5—Cl4—C47—Cl7 | 75.57 | C45—C21—C22—C1 | −1.60 |
Cl5—Cl4—C48—Cl7 | 82.35 | C45—C21—C22—C8 | −179.77 |
C47—Cl4—Cl5—C48 | 1.25 | C31—C21—C22—C1 | −126.69 |
C48—Cl4—Cl5—C47 | −1.25 | C31—C21—C22—C8 | 55.14 |
C48—Cl4—C47—Cl8 | 76.54 | C45—C21—C31—C33 | −4.66 |
Cl5—Cl4—C47—C48 | −14.48 | C22—C21—C31—C29 | −55.95 |
C47—Cl4—C48—Cl2 | 23.43 | C22—C21—C31—C33 | 124.71 |
C47—Cl4—C48—Cl1 | 19.26 | C18—C21—C31—C33 | −124.05 |
Cl5—Cl4—C48—Cl2 | −170.64 | C18—C21—C22—C8 | −55.23 |
Cl5—Cl4—C47—Cl8 | 62.06 | C45—C21—C31—C29 | 174.68 |
C47—Cl4—C48—Cl5 | −165.93 | C18—C21—C22—C1 | 122.95 |
C48—Cl4—C47—Cl7 | 90.04 | C29—C25—C26—C11 | −124.81 |
Cl4—Cl5—C48—Cl1 | 5.77 | C8—C25—C26—C18 | −57.44 |
C48—Cl5—C47—Cl7 | 86.46 | C26—C25—C29—C39 | 123.08 |
Cl4—Cl5—C47—Cl8 | −120.73 | C8—C25—C26—C11 | 122.27 |
C48—Cl5—C47—Cl8 | 73.42 | C29—C25—C26—C18 | 55.48 |
Cl4—Cl5—C47—C48 | 165.84 | C8—C25—C29—C39 | −124.54 |
Cl4—Cl5—C48—Cl8 | −113.56 | C26—C25—C29—C31 | −56.40 |
Cl4—Cl5—C48—C47 | −13.55 | C8—C25—C29—C31 | 55.98 |
Cl4—Cl5—C47—Cl7 | −107.70 | C25—C29—C31—C33 | 179.51 |
Cl4—Cl5—C48—Cl7 | −100.91 | C25—C29—C31—C21 | 0.12 |
C47—Cl5—C48—Cl7 | −87.36 | C39—C29—C31—C33 | 0 |
Cl4—Cl5—C47—Cl1 | 8.99 | C39—C29—C31—C21 | −179.40 |
C48—Cl5—C47—Cl1 | −156.85 | C31—C29—C39—C37 | 0.44 |
C48—Cl5—C47—Cl4 | −165.84 | C25—C29—C39—C37 | −179.01 |
C47—Cl5—C48—Cl8 | −100.01 | C21—C31—C33—C35 | 178.63 |
C48—Cl5—C47—Cl2 | −154.05 | C29—C31—C33—C35 | −0.66 |
C47—Cl5—C48—Cl4 | 13.55 | C31—C33—C35—C37 | 0.92 |
Cl4—Cl5—C48—Cl2 | 9.66 | C33—C35—C37—C39 | −0.50 |
C47—Cl5—C48—Cl2 | 23.21 | C35—C37—C39—C29 | −0.18 |
Cl4—Cl5—C47—Cl2 | 11.79 | Cl8—C47—C48—Cl7 | 1.97 |
C47—Cl5—C48—Cl1 | 19.32 | Cl8—C47—C48—Cl4 | −107.45 |
Cl8—Cl7—C48—Cl4 | −98.86 | Cl8—C47—C48—Cl5 | −104.91 |
C47—Cl7—C48—Cl4 | 71.94 | Cl1—C47—C48—Cl2 | 24.14 |
C47—Cl7—C48—Cl2 | −28.36 | Cl1—C47—C48—Cl4 | 155.45 |
Cl8—Cl7—C48—Cl1 | 143.36 | Cl1—C47—C48—Cl5 | 157.98 |
C47—Cl7—C48—Cl1 | −45.84 | Cl1—C47—C48—Cl7 | −95.14 |
Cl8—Cl7—C48—Cl2 | 160.85 | Cl1—C47—C48—Cl8 | −97.11 |
Cl8—Cl7—C47—Cl5 | −82.50 | Cl2—C47—C48—Cl1 | −24.14 |
C48—Cl7—C47—Cl5 | −91.13 | Cl2—C47—C48—Cl4 | 131.3 |
Cl8—Cl7—C48—Cl5 | −88.08 | Cl2—C47—C48—Cl5 | 133.84 |
Cl8—Cl7—C47—C48 | 8.63 | Cl2—C47—C48—Cl7 | −119.28 |
C47—Cl7—C48—Cl5 | 82.72 | Cl2—C47—C48—Cl8 | −121.25 |
C47—Cl7—C48—Cl8 | 170.8 | Cl4—C47—C48—Cl1 | −155.45 |
Cl8—Cl7—C48—C47 | −170.80 | Cl4—C47—C48—Cl2 | −131.30 |
C48—Cl7—C47—Cl4 | −101.45 | Cl4—C47—C48—Cl5 | 2.54 |
C47—Cl7—Cl8—C48 | −0.92 | Cl4—C47—C48—Cl7 | 109.42 |
C48—Cl7—Cl8—C47 | 0.92 | Cl4—C47—C48—Cl8 | 107.45 |
Cl8—Cl7—C47—Cl1 | 138.52 | Cl5—C47—C48—Cl1 | −157.98 |
C48—Cl7—C47—Cl2 | 148.4 | Cl5—C47—C48—Cl2 | −133.84 |
C48—Cl7—C47—Cl1 | 129.89 | Cl5—C47—C48—Cl4 | −2.54 |
Cl8—Cl7—C47—Cl2 | 157.03 | Cl5—C47—C48—Cl7 | 106.88 |
C48—Cl7—C47—Cl8 | −8.63 | Cl5—C47—C48—Cl8 | 104.91 |
Cl8—Cl7—C47—Cl4 | −92.83 | Cl7—C47—C48—Cl1 | 95.14 |
C48—Cl8—C47—Cl7 | 171.02 | Cl7—C47—C48—Cl2 | 119.28 |
C48—Cl8—C47—Cl2 | 145.57 | Cl7—C47—C48—Cl4 | −109.42 |
Cl7—Cl8—C47—Cl2 | −25.45 | Cl7—C47—C48—Cl5 | −106.88 |
Cl7—Cl8—C47—Cl4 | 91.78 | Cl7—C47—C48—Cl8 | −1.97 |
C48—Cl8—C47—Cl4 | −97.20 | Cl8—C47—C48—Cl1 | 97.11 |
Cl7—Cl8—C47—Cl5 | 101.09 | Cl8—C47—C48—Cl2 | 121.25 |
C48—Cl8—C47—Cl5 | −87.89 | | |
Symmetry codes: (i) −x, −y+2, −z; (ii) −x, −y+2, −z+1; (iii) x+1/2, −y+3/2, z+1/2; (iv) x−1/2, −y+3/2, z−1/2; (v) −x+1/2, y−1/2, −z+1/2; (vi) −x+1/2, y+1/2, −z+1/2. |
(29) tris(1,2-Di-imidobenzene)-technetium(vii) pertechnetate
top
Crystal data top
C18H18N6Tc+·O4Tc− | Z = 4 |
Mr = 580.20 | F(000) = 944 |
Orthorhombic, Pnna | Dx = 1.718 Mg m−3 |
Hall symbol: -P 2a 2bc | Mo Kα radiation, λ = 0.71070 Å |
a = 13.869 (4) Å | µ = 1.45 mm−1 |
b = 10.851 (3) Å | T = 293 K |
c = 12.799 (5) Å | × × mm |
V = 1926.2 (11) Å3 | |
Data collection top
Radiation source: fine-focus sealed tube | θmax = 40.0°, θmin = 2.2° |
18522 measured reflections | h = −14→14 |
2456 independent reflections | k = −12→12 |
2454 reflections with I > 2σ(I) | l = −13→13 |
Rint = 0.003 | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.606 | w = 1/[σ2(Fo2) + (0.2P)2] where P = (Fo2 + 2Fc2)/3 |
S = 3.25 | (Δ/σ)max = 0.551 |
2456 reflections | Δρmax = 1.20 e Å−3 |
52 parameters | Δρmin = −3.52 e Å−3 |
0 restraints | Extinction correction: nne |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
C18H18N6Tc+·O4Tc− | V = 1926.2 (11) Å3 |
Mr = 580.20 | Z = 4 |
Orthorhombic, Pnna | Mo Kα radiation |
a = 13.869 (4) Å | µ = 1.45 mm−1 |
b = 10.851 (3) Å | T = 293 K |
c = 12.799 (5) Å | × × mm |
Data collection top
18522 measured reflections | 2454 reflections with I > 2σ(I) |
2456 independent reflections | Rint = 0.003 |
Refinement top
R[F2 > 2σ(F2)] = 0.122 | 0 restraints |
wR(F2) = 0.606 | H atoms treated by a mixture of independent and constrained refinement |
S = 3.25 | (Δ/σ)max = 0.551 |
2456 reflections | Δρmax = 1.20 e Å−3 |
52 parameters | Δρmin = −3.52 e Å−3 |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is nt relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Tc1 | 0.5069 | 0.75 | 0.25 | 0.02* | |
N1 | 0.45455 | 0.717 | 0.10655 | 0.02* | |
N2 | 0.4453 | 0.583 | 0.26345 | 0.02* | |
N5 | 0.62105 | 0.82545 | 0.17815 | 0.02* | |
C1 | 0.4178 | 0.6039 | 0.08625 | 0.02* | |
C2 | 0.3876 | 0.5574 | −0.01130 | 0.02* | |
C3 | 0.35385 | 0.4435 | −0.02180 | 0.02* | |
C4 | 0.344 | 0.3623 | 0.0721 | 0.02* | |
C5 | 0.3737 | 0.4057 | 0.16965 | 0.02* | |
C6 | 0.4116 | 0.53015 | 0.1766 | 0.02* | |
C13 | 0.7108 | 0.79425 | 0.207 | 0.02* | |
C14 | 0.7985 | 0.83635 | 0.16865 | 0.02* | |
C15 | 0.8846 | 0.7941 | 0.20855 | 0.02* | |
Tc2 | 0 | 0 | 0 | 0.02* | |
Geometric parameters (Å, º) top
Tc1—N1 | 2.0066 | C2—C3 | 1.3284 |
Tc1—N2 | 2.0108 | C3—C4 | 1.4965 |
Tc1—N5 | 2.0056 | C4—C5 | 1.3965 |
N1—C1 | 1.354 | C5—C6 | 1.4518 |
N2—C6 | 1.3353 | C13—C14 | 1.3889 |
N5—C13 | 1.3418 | C13—C13i | 1.4607 |
C1—C2 | 1.4103 | C14—C15 | 1.3773 |
C1—C6 | 1.4089 | C15—C15i | 1.4289 |
| | | |
Tc1···Tc2ii | 4.1960 (16) | N1···C3x | 3.3572 |
Tc1···Tc2iii | 4.1960 (16) | N2···Tc2iii | 3.2485 |
Tc1···Tc2iv | 4.1960 (16) | N2···Tc2v | 3.2485 |
Tc1···Tc2v | 4.1960 (16) | N5···Tc2iv | 3.4066 |
Tc2···Tc1vi | 4.1960 (16) | N5···Tc2ii | 3.4066 |
Tc2···N1vi | 3.4186 | C1···C2x | 3.3567 |
Tc2···N5vi | 3.4066 | C1···C3x | 3.3128 |
Tc2···Tc1vii | 4.1960 (16) | C2···C3ii | 3.3514 |
Tc2···N2vii | 3.2485 | C2···C2x | 3.3698 |
Tc2···Tc1viii | 4.1960 (16) | C2···C4ii | 3.4951 |
Tc2···N2viii | 3.2485 | C2···C1x | 3.3567 |
Tc2···C14ix | 3.9525 | C3···C2ii | 3.3514 |
Tc2···C15ix | 3.8312 | C3···C1x | 3.3128 |
Tc2···Tc1ii | 4.1960 (16) | C3···C3ii | 3.1307 |
Tc2···N1ii | 3.4186 | C3···N1x | 3.3572 |
Tc2···N5ii | 3.4066 | C4···C2ii | 3.4951 |
Tc2···C15x | 3.8312 | C14···Tc2x | 3.9525 |
Tc2···C14x | 3.9525 | C14···Tc2xi | 3.9525 |
N1···Tc2ii | 3.4186 | C15···Tc2x | 3.8312 |
N1···Tc2iv | 3.4186 | C15···Tc2xi | 3.8312 |
| | | |
N1—Tc1—N2 | 76.34 | Tc1—N5—C13 | 120.21 |
N1—Tc1—N5 | 86.5 | N1—C1—C2 | 127.3 |
N1—Tc1—N1i | 137.57 | N1—C1—C6 | 112.35 |
N1—Tc1—N2i | 85.91 | C2—C1—C6 | 120.35 |
N1—Tc1—N5i | 129.22 | C1—C2—C3 | 121.81 |
N2—Tc1—N5 | 137.95 | C2—C3—C4 | 119.92 |
N1i—Tc1—N2 | 85.91 | C3—C4—C5 | 119.51 |
N2—Tc1—N2i | 129.71 | C4—C5—C6 | 118.37 |
N2—Tc1—N5i | 85.89 | N2—C6—C1 | 114.71 |
N1i—Tc1—N5 | 129.22 | N2—C6—C5 | 125.25 |
N2i—Tc1—N5 | 85.89 | C1—C6—C5 | 120.01 |
N5—Tc1—N5i | 75.75 | N5—C13—C14 | 129.21 |
N1i—Tc1—N2i | 76.34 | N5—C13—C13i | 111.92 |
N1i—Tc1—N5i | 86.5 | C13i—C13—C14 | 118.85 |
N2i—Tc1—N5i | 137.95 | C13—C14—C15 | 121.25 |
Tc1—N1—C1 | 118.26 | C14—C15—C15i | 119.89 |
Tc1—N2—C6 | 117.68 | | |
| | | |
N2—Tc1—N1—C1 | −7.54 | Tc1—N5—C13—C14 | −179.14 |
N5—Tc1—N1—C1 | 133.76 | C6—C1—C2—C3 | −0.88 |
N1i—Tc1—N1—C1 | −75.54 | N1—C1—C6—N2 | −1.97 |
N2i—Tc1—N1—C1 | −140.12 | N1—C1—C6—C5 | 179.94 |
N5i—Tc1—N1—C1 | 65.38 | N1—C1—C2—C3 | 178.98 |
N1—Tc1—N2—C6 | 6.31 | C2—C1—C6—N2 | 177.91 |
N5—Tc1—N2—C6 | −62.38 | C2—C1—C6—C5 | −0.18 |
N1i—Tc1—N2—C6 | 147.48 | C1—C2—C3—C4 | 2.07 |
N2i—Tc1—N2—C6 | 79.02 | C2—C3—C4—C5 | −2.27 |
N5i—Tc1—N2—C6 | −125.75 | C3—C4—C5—C6 | 1.22 |
N1—Tc1—N5—C13 | −131.64 | C4—C5—C6—N2 | −177.94 |
N2—Tc1—N5—C13 | −66.55 | C4—C5—C6—C1 | −0.07 |
N1i—Tc1—N5—C13 | 73.58 | N5—C13—C14—C15 | 179.61 |
N2i—Tc1—N5—C13 | 142.21 | C13i—C13—C14—C15 | 1.5 |
N5i—Tc1—N5—C13 | 0.36 | N5—C13—C13i—N5i | 1.14 |
Tc1—N1—C1—C2 | −172.36 | N5—C13—C13i—C14i | 179.55 |
Tc1—N1—C1—C6 | 7.5 | C14—C13—C13i—N5i | 179.55 |
Tc1—N2—C6—C1 | −4.33 | C14—C13—C13i—C14i | −2.03 |
Tc1—N2—C6—C5 | 173.64 | C13—C14—C15—C15i | −0.43 |
Tc1—N5—C13—C13i | −0.93 | C14—C15—C15i—C14i | −0.15 |
Symmetry codes: (i) x, −y+3/2, −z+1/2; (ii) −x+1/2, −y+1, z; (iii) −x+1/2, y+1/2, −z+1/2; (iv) x+1/2, y+1, −z; (v) x+1/2, −y+1/2, z+1/2; (vi) x−1/2, y−1, −z; (vii) x−1/2, −y+1/2, z−1/2; (viii) −x+1/2, y−1/2, −z+1/2; (ix) x−1, y−1, z; (x) −x+1, −y+1, −z; (xi) x+1, y+1, z. |
(30) bis(n-propylamine)dichloropalladium(II)
top
Crystal data top
C6H18Cl2N2Pd | γ = 90° |
Mr = 295.54 | V = 567.6 (2) Å3 |
Monclinic, C2/m | Z = 2 |
Hall symbol: -C 2y | F(000) = 296 |
a = 8.929 (2) Å | Dx = 1.729 Mg m−3 |
b = 8.437 (2) Å | Mo K\a radiation, λ = 0.71070 Å |
c = 7.542 (2) Å | µ = 2.06 mm−1 |
α = 90° | T = 0 K |
β = 92.65 (3)° | × × mm |
Crystal data top
C6H18Cl2N2Pd | γ = 90° |
Mr = 295.54 | V = 567.6 (2) Å3 |
Monclinic, C2/m | Z = 2 |
a = 8.929 (2) Å | Mo K\a radiation |
b = 8.437 (2) Å | µ = 2.06 mm−1 |
c = 7.542 (2) Å | T = 0 K |
α = 90° | × × mm |
β = 92.65 (3)° | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Pd1 | 0 | 0 | 1 | 0.02* | |
Cl1 | 0 | 0.272 | 1 | 0.02* | |
N1 | 0.1963 | 0 | 0.8671 | 0.02* | |
C1 | 0.1661 | 0 | 0.67330 | 0.02* | |
C2 | 0.3076 | 0 | 0.569 | 0.02* | |
C3 | 0.2705 | 0 | 0.3725 | 0.02* | |
H1 | 0.25054 | 0.08630 | 0.89844 | 0.02* | |
H2 | 0.10700 | 0.09286 | 0.64064 | 0.02* | |
H3 | 0.36696 | 0.09303 | 0.60024 | 0.02* | |
H4 | 0.36158 | 0 | 0.30969 | 0.02* | |
H5 | 0.21400 | 0.09346 | 0.34099 | 0.02* | |
Geometric parameters (Å, º) top
Pd1—Cl1 | 2.2949 (6) | C1—C2 | 1.5189 (4) |
Pd1—N1 | 2.0590 (5) | C2—C3 | 1.5036 (4) |
Pd1—N1i | 2.0590 (5) | C1—H2 | 0.97 |
Pd1—Cl1ii | 2.2949 (6) | C2—H3 | 0.97 |
N1—C1 | 1.4740 (4) | C3—H4 | 0.96 |
N1—H1 | 0.9 | C3—H5 | 0.96 |
| | | |
Pd1···C3iii | 3.6192 (10) | C3···Pd1v | 3.6192 (10) |
Pd1···C3iv | 3.6192 (10) | C3···Pd1iv | 3.6192 (10) |
Pd1···C3v | 3.6192 (10) | C3···Pd1xiv | 3.6192 (10) |
Pd1···C3vi | 3.6192 (10) | C3···Pd1xv | 3.6192 (10) |
Pd1···H5iii | 3.2299 | C2···H4xvi | 3.0516 |
Pd1···H5iv | 3.2299 | C2···H4xvii | 3.0516 |
Pd1···H5v | 3.2299 | H1···H3 | 2.5215 |
Pd1···H5vi | 3.2299 | H1···Cl1ix | 2.6115 |
Cl1···N1vii | 3.4362 (9) | H1···Cl1xiii | 2.6115 |
Cl1···N1viii | 3.4362 (9) | H2···H5 | 2.494 |
Cl1···N1ix | 3.4362 (9) | H3···H1 | 2.5215 |
Cl1···N1x | 3.4362 (9) | H4···C2xvi | 3.0516 |
Cl1···H1ix | 2.6115 | H4···C2xvii | 3.0516 |
Cl1···H1x | 2.6115 | H5···Pd1xiv | 3.2299 |
N1···Cl1xi | 3.4362 (9) | H5···H2 | 2.494 |
N1···Cl1xii | 3.4362 (9) | H5···Pd1v | 3.2299 |
N1···Cl1ix | 3.4362 (9) | H5···Pd1iv | 3.2299 |
N1···Cl1xiii | 3.4362 (9) | H5···Pd1xv | 3.2299 |
| | | |
Cl1—Pd1—N1 | 90.00 (3) | N1—C1—H2xviii | 108.92 |
Cl1—Pd1—N1i | 90.00 (3) | C2—C1—H2 | 108.92 |
Cl1—Pd1—Cl1ii | 180 | C2—C1—H2xviii | 108.92 |
N1—Pd1—N1i | 180 | H2—C1—H2xviii | 107.74 |
Cl1ii—Pd1—N1 | 90.00 (3) | C1—C2—H3 | 109.42 |
Cl1ii—Pd1—N1i | 90.00 (3) | C1—C2—H3xviii | 109.42 |
Pd1—N1—C1 | 111.22 (3) | C3—C2—H3 | 109.42 |
Pd1—N1—H1xviii | 109.39 | C3—C2—H3xviii | 109.42 |
C1—N1—H1 | 109.39 | H3—C2—H3xviii | 108.02 |
Pd1—N1—H1 | 109.39 | C2—C3—H4 | 109.47 |
H1—N1—H1xviii | 108.01 | C2—C3—H5 | 109.47 |
C1—N1—H1xviii | 109.39 | C2—C3—H5xviii | 109.47 |
N1—C1—C2 | 113.27 (3) | H4—C3—H5 | 108.99 |
C1—C2—C3 | 111.09 (3) | H4—C3—H5xviii | 108.99 |
N1—C1—H2 | 108.92 | H5—C3—H5xviii | 110.44 |
| | | |
Cl1—Pd1—N1—C1 | −90.00 (3) | N1—C1—C2—C3 | −180.00 (3) |
Pd1—N1—C1—C2 | 180.00 (3) | | |
Symmetry codes: (i) −x, y, −z+2; (ii) −x, −y, −z+2; (iii) x, y, z+1; (iv) −x, −y, −z+1; (v) −x, y, −z+1; (vi) x, −y, z+1; (vii) x−1/2, y+1/2, z; (viii) −x+1/2, y+1/2, −z+2; (ix) −x+1/2, −y+1/2, −z+2; (x) x−1/2, −y+1/2, z; (xi) x+1/2, y−1/2, z; (xii) −x+1/2, y−1/2, −z+2; (xiii) x+1/2, −y+1/2, z; (xiv) x, y, z−1; (xv) x, −y, z−1; (xvi) −x+1, y, −z+1; (xvii) −x+1, −y, −z+1; (xviii) x, −y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···Cl1ix | 0.9 | 2.61 | 3.4362 (9) | 153 |
N1—H1···Cl1xiii | 0.9 | 2.61 | 3.4362 (9) | 153 |
Symmetry codes: (ix) −x+1/2, −y+1/2, −z+2; (xiii) x+1/2, −y+1/2, z. |
Experimental details
| (1) | (2) | (3) | (4) |
Crystal data |
Chemical formula | C10H12CuN2O6S | C8H20CoN6O4·H2O·Cl | C23H39N5O4Si2 | C20H30O2 |
Mr | 351.84 | 376.70 | 505.77 | 302.44 |
Crystal system, space group | Monclinic, I2/a | Orthorhombic, Cmc21 | Orthorhombic, C2221 | Monclinic, I2/a |
Temperature (K) | 0 | 293 | 0 | 0 |
a, b, c (Å) | 6.963 (1), 12.4686 (16), 14.8540 (15) | 9.515 (7), 11.909 (9), 13.003 (10) | 13.1422 (15), 12.1676 (15), 34.638 (4) | 27.869 (1), 5.771 (3), 11.758 (5) |
α, β, γ (°) | 90, 101.01 (1), 90 | 90, 90, 90 | 90, 90, 90 | 90, 91.43 (1), 90 |
V (Å3) | 1265.9 (3) | 1473.4 (19) | 5538.9 (11) | 1890.5 (13) |
Z | 4 | 4 | 8 | 4 |
Radiation type | Mo K\a | Mo Kα | Mo K\a | Mo K\a |
µ (mm−1) | 1.92 | 1.38 | 0.16 | 0.06 |
Crystal size (mm) | × × | × × | × × | × × |
|
Data collection |
Diffractometer | ? | ? | ? | ? |
Absorption correction | – | – | – | – |
No. of measured, independent and observed reflections | ?, ?, ? (?) | 1146, 654, 652 [I > 2σ(I)] | ?, ?, ? (?) | ?, ?, ? (?) |
Rint | ? | 0.037 | ? | ? |
Distance from source to specimen (mm) | – | 0.596 | – | – |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? | 0.028, 0.088, 1.46 | ?, ?, ? | ?, ?, ? |
No. of reflections | ? | 654 | ? | ? |
No. of parameters | ? | 118 | ? | ? |
No. of restraints | 0 | 2 | 0 | 0 |
H-atom treatment | See text | H atoms treated by a mixture of independent and constrained refinement | See text | See text |
| ? | w = 1/[σ2(Fo2) + (0.P)2 + 3.9018P] where P = (Fo2 + 2Fc2)/3 | ? | ? |
(Δ/σ)max | ? | 0.008 | ? | ? |
Δρmax, Δρmin (e Å−3) | ?, ? | 0.28, −0.32 | ?, ? | ?, ? |
Absolute structure | ? | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H.D. (1983), Acta Cryst. A39, 876-881 | ? |
Absolute structure parameter | nne | −0.01 (7) | ? | nne |
| (5) | (6) | (7) | (8) |
Crystal data |
Chemical formula | C23H32ClCuN4+·Cl−·H2O | C32H38CaN4O12S2 | 2(C12IrN8O2−)·(C12N10Pt−)·3(C7H18N+)·3(C2H3N) | C13H12ClNO4 |
Mr | 514.98 | 774.88 | see text | 281.69 |
Crystal system, space group | Monclinic, I2/a | Orthorhombic, C2221 | Orthorhombic, Cmc21 | Orthorhombic, Cmca |
Temperature (K) | 0 | 0 | 0 | 0 |
a, b, c (Å) | 18.6300 (18), 16.610 (2), 16.972 (3) | 19.036 (10), 6.508 (2), 29.178 (18) | 15.151 (19), 22.13 (2), 6.874 (5) | 6.707 (1), 17.023 (4), 22.938 (2) |
α, β, γ (°) | 90, 108.020 (9), 90 | 90, 90, 90 | 90, 90, 90 | 90, 90, 90 |
V (Å3) | 4994.3 (12) | 3615 (3) | 2305 (4) | 2618.9 (8) |
Z | 8 | 4 | 4 | 8 |
Radiation type | Mo K\a | Mo K\a | Mo K\a | Mo K\a |
µ (mm−1) | 1.11 | 0.35 | 6.13 | 0.30 |
Crystal size (mm) | × × | × × | × × | × × |
|
Data collection |
Diffractometer | ? | ? | ? | ? |
Absorption correction | – | – | – | – |
No. of measured, independent and observed reflections | ?, ?, ? (?) | ?, ?, ? (?) | ?, ?, ? (?) | ?, ?, ? (?) |
Rint | ? | ? | ? | ? |
Distance from source to specimen (mm) | – | – | – | – |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? | ?, ?, ? | ?, ?, ? | ?, ?, ? |
No. of reflections | ? | ? | ? | ? |
No. of parameters | ? | ? | ? | ? |
No. of restraints | 0 | 0 | 0 | 0 |
H-atom treatment | See text | See text | See text | See text |
| ? | ? | ? | ? |
(Δ/σ)max | ? | ? | ? | ? |
Δρmax, Δρmin (e Å−3) | ?, ? | ?, ? | ?, ? | ?, ? |
Absolute structure | ? | Flack H.D. (1983), Acta Cryst. A39, 876-881 | Flack H.D. (1983), Acta Cryst. A39, 876-881 | ? |
Absolute structure parameter | nne | ? | ? | nne |
| (9) | (10) | (11) | (12) |
Crystal data |
Chemical formula | C10H12N4O8P·2.5(H2O)·8(H2O) | C18H22N2O8Zn2 | C10H18FeN2O4·2(C2H3O2) | F6P·C10H24N4O2Re |
Mr | 536.38 | 525.16 | 404.20 | 563.49 |
Crystal system, space group | Orthorhombic, C2221 | Monclinic, P21/n | Monclinic, I2/m | Monclinic, I2/a |
Temperature (K) | 0 | 0 | 0 | 293 |
a, b, c (Å) | 23.1914 (10), 8.650 (1), 21.900 (1) | 8.626 (2), 28.871 (8), 8.868 (3) | 11.780 (2), 9.734 (2), 8.401 (2) | 17.257 (4), 5.533 (1), 18.053 (4) |
α, β, γ (°) | 90, 90, 90 | 90, 99.02 (2), 90 | 90, 104.05 (2), 90 | 90, 98.14 (2), 90 |
V (Å3) | 4393.3 (6) | 2181.2 (11) | 934.5 (3) | 1706.4 (6) |
Z | 8 | 4 | 2 | 4 |
Radiation type | Mo K\a | Mo K\a | Mo K\a | Mo Kα |
µ (mm−1) | 0.22 | 2.24 | 0.85 | 7.29 |
Crystal size (mm) | × × | × × | × × | × × |
|
Data collection |
Diffractometer | ? | ? | ? | ? |
Absorption correction | – | – | – | – |
No. of measured, independent and observed reflections | ?, ?, ? (?) | ?, ?, ? (?) | ?, ?, ? (?) | 4752, 2500, 2150 [I > 2σ(I)] |
Rint | ? | ? | ? | 0.121 |
Distance from source to specimen (mm) | – | – | – | 0.705 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? | ?, ?, ? | ?, ?, ? | 0.077, 0.192, 1.32 |
No. of reflections | ? | ? | ? | 2500 |
No. of parameters | ? | ? | ? | 129 |
No. of restraints | 0 | 0 | 0 | 1 |
H-atom treatment | See text | See text | See text | H atoms treated by a mixture of independent and constrained refinement |
| ? | ? | ? | w = 1/[σ2(Fo2) + (0.069P)2 + 29.4858P] where P = (Fo2 + 2Fc2)/3 |
(Δ/σ)max | ? | ? | ? | 0.001 |
Δρmax, Δρmin (e Å−3) | ?, ? | ?, ? | ?, ? | 5.90, −4.02 |
Absolute structure | Flack H.D. (1983), Acta Cryst. A39, 876-881 | ? | ? | ? |
Absolute structure parameter | ? | nne | nne | ? |
| (13) | (14) | (15) | (16) |
Crystal data |
Chemical formula | C60H120Fe6N12O24 | C96H80P4Pd·4(C6H6) | C19H22Cl2CuN6O5S4 | C14H14CdN2O5·2(H2O) |
Mr | 1728.78 | 1776.33 | 677.16 | 438.71 |
Crystal system, space group | Orthorhombic, Ccca | Orthorhombic, C2221 | Monclinic, I2/a | Monclinic, C2/c |
Temperature (K) | 0 | 0 | 293 | 0 |
a, b, c (Å) | 20.939 (2), 25.243 (4), 16.048 (1) | 29.327 (12), 16.743 (7), 19.458 (6) | 30.123 (13), 7.564 (6), 11.044 (6) | 15.2963 (19), 6.2028 (7), 17.8150 (18) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 91.27 (1), 90 | 90, 106.196 (4), 90 |
V (Å3) | 8482.4 (17) | 9554 (6) | 2516 (3) | 1623.2 (3) |
Z | 4 | 4 | 4 | 4 |
Radiation type | Mo K\a | Mo K\a | Mo Kα | Mo K\a |
µ (mm−1) | 1.07 | 0.31 | 1.46 | 1.38 |
Crystal size (mm) | × × | × × | × × | × × |
|
Data collection |
Diffractometer | ? | ? | ? | ? |
Absorption correction | – | – | – | – |
No. of measured, independent and observed reflections | ?, ?, ? (?) | ?, ?, ? (?) | 3814, 2078, 2062 [I > 2σ(I)] | ?, ?, ? (?) |
Rint | ? | ? | 0.069 | ? |
Distance from source to specimen (mm) | – | – | 0.653 | – |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? | ?, ?, ? | 0.053, 0.156, 1.16 | ?, ?, ? |
No. of reflections | ? | ? | 2078 | ? |
No. of parameters | ? | ? | 173 | ? |
No. of restraints | 0 | 0 | 0 | 0 |
H-atom treatment | See text | See text | H atoms treated by a mixture of independent and constrained refinement | See text |
| ? | ? | w = 1/[σ2(Fo2) + (0.0576P)2 + 14.5807P] where P = (Fo2 + 2Fc2)/3 | ? |
(Δ/σ)max | ? | ? | < 0.001 | ? |
Δρmax, Δρmin (e Å−3) | ?, ? | ?, ? | 0.70, −0.90 | ?, ? |
Absolute structure | ? | Flack H.D. (1983), Acta Cryst. A39, 876-881 | ? | ? |
Absolute structure parameter | nne | ? | ? | nne |
| (17) | (18) | (19) | (20) |
Crystal data |
Chemical formula | C20H15FeNO2 | C10H24Cl2Mg2O8·C10H20MgO6·4(Cl) | C12N6O12Re3 | C10H7N3S2 |
Mr | 357.18 | 794.18 | 978.81 | 233.33 |
Crystal system, space group | Monclinic, P21/n | Orthorhombic, Pmna | Orthorhombic, Pnma | Monclinic, P21/m |
Temperature (K) | 0 | 0 | 0 | 0 |
a, b, c (Å) | 10.391 (2), 7.252 (3), 20.662 (2) | 13.303 (3), 7.835 (2), 18.169 (4) | 20.639 (3), 16.657 (3), 6.705 (3) | 5.628 (1), 7.207 (2), 13.126 (2) |
α, β, γ (°) | 90, 97.47 (2), 90 | 90, 90, 90 | 90, 90, 90 | 90, 100.12 (6), 90 |
V (Å3) | 1543.8 (7) | 1893.7 (8) | 2305.1 (12) | 524.1 (2) |
Z | 4 | 2 | 4 | 2 |
Radiation type | Mo K\a | Mo Kα | Mo K\a | Mo K\a |
µ (mm−1) | 0.99 | 0.55 | 15.78 | 0.47 |
Crystal size (mm) | × × | × × | × × | × × |
|
Data collection |
Diffractometer | ? | ? | ? | ? |
Absorption correction | – | – | – | – |
No. of measured, independent and observed reflections | ?, ?, ? (?) | 16258, 2204, 1626 [I > 2σ(I)] | ?, ?, ? (?) | ?, ?, ? (?) |
Rint | ? | 0.274 | ? | ? |
Distance from source to specimen (mm) | – | 0.863 | – | – |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? | 0.129, 0.473, 2.65 | ?, ?, ? | ?, ?, ? |
No. of reflections | ? | 2204 | ? | ? |
No. of parameters | ? | 54 | ? | ? |
No. of restraints | 0 | 0 | 0 | 0 |
H-atom treatment | See text | H atoms treated by a mixture of independent and constrained refinement | – | See text |
| ? | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 | ? | ? |
(Δ/σ)max | ? | 0.593 | ? | ? |
Δρmax, Δρmin (e Å−3) | ?, ? | ?, ? | ?, ? | ?, ? |
Absolute structure | ? | ? | ? | ? |
Absolute structure parameter | nne | ? | nne | nne |
| (21) | (22) | (23) | (25) |
Crystal data |
Chemical formula | C2Cl4O2Pt2 | C7H9NO2 | C38H33Cl2N2P2ReS2 | (C12H12Cr+)·(OH−)·3(H2O) |
Mr | 587.98 | 139.15 | 900.86 | 279.28 |
Crystal system, space group | Tetragonal, P42/m | Monclinic, P21/m | Monclinic, C2/c | Orthorhombic, Cmca |
Temperature (K) | 0 | 0 | 0 | 0 |
a, b, c (Å) | 11.183 (3), 11.183 (3), 3.525 (2) | 7.110 (4), 6.993 (4), 7.678 (4) | 17.514 (4), 10.639 (2), 20.106 (4) | 16.409 (3), 10.506 (4), 7.825 (3) |
α, β, γ (°) | 90, 90, 90 | 90, 117.04 (4), 90 | 90, 102.29 (3), 90 | 90, 90, 90 |
V (Å3) | 440.8 (3) | 340.0 (3) | 3660.5 (14) | 1349.0 (8) |
Z | 2 | 2 | 4 | 4 |
Radiation type | Mo K\a | Mo K\a | Mo Kα | Mo K\a |
µ (mm−1) | 32.85 | 0.10 | 3.70 | 0.85 |
Crystal size (mm) | × × | × × | × × | × × |
|
Data collection |
Diffractometer | ? | ? | ? | ? |
Absorption correction | – | – | – | – |
No. of measured, independent and observed reflections | ?, ?, ? (?) | ?, ?, ? (?) | 17044, 4363, 4277 [I > 2σ(I)] | ?, ?, ? (?) |
Rint | ? | ? | 0.022 | ? |
Distance from source to specimen (mm) | – | – | 0.938 | – |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? | ?, ?, ? | 0.049, 0.259, 1.18 | ?, ?, ? |
No. of reflections | ? | ? | 4363 | ? |
No. of parameters | ? | ? | 105 | ? |
No. of restraints | 0 | 0 | 0 | 0 |
H-atom treatment | – | See text | H atoms treated by a mixture of independent and constrained refinement | See text |
| ? | ? | w = 1/[σ2(Fo2) + (0.2P)2] where P = (Fo2 + 2Fc2)/3 | ? |
(Δ/σ)max | ? | ? | 0.946 | ? |
Δρmax, Δρmin (e Å−3) | ?, ? | ?, ? | 2.01, −2.68 | ?, ? |
Absolute structure | ? | ? | ? | ? |
Absolute structure parameter | nne | nne | ? | nne |
| (26) | (27) | (28) | (29) |
Crystal data |
Chemical formula | C12H23Cl3NP2Re | C12H13Ir3 | C46H34·2(CHCl3) | C18H18N6Tc+·O4Tc− |
Mr | 535.80 | 733.88 | 825.47 | 580.20 |
Crystal system, space group | Orthorhombic, Cmcm | Orthorhombic, Cmcm | Monclinic, P21/n | Orthorhombic, Pnna |
Temperature (K) | 0 | 0 | 0 | 293 |
a, b, c (Å) | 11.0341 (10), 16.814 (2), 10.844 (1) | 11.2624, 9.711, 25.998 | 15.592 (2), 8.642 (2), 16.677 (2) | 13.869 (4), 10.851 (3), 12.799 (5) |
α, β, γ (°) | 90, 90, 90 | 90, 90, 90 | 90, 114.773 (9), 90 | 90, 90, 90 |
V (Å3) | 2011.9 (4) | 2843.38 | 2040.4 (6) | 1926.2 (11) |
Z | 4 | 4 | 2 | 4 |
Radiation type | Mo K\a | Mo K\a | Mo K\a | Mo Kα |
µ (mm−1) | 6.58 | 13.99 | 0.45 | 1.45 |
Crystal size (mm) | × × | × × | × × | × × |
|
Data collection |
Diffractometer | ? | ? | ? | ? |
Absorption correction | – | – | – | – |
No. of measured, independent and observed reflections | ?, ?, ? (?) | ?, ?, ? (?) | ?, ?, ? (?) | 18522, 2456, 2454 [I > 2σ(I)] |
Rint | ? | ? | ? | 0.003 |
Distance from source to specimen (mm) | – | – | – | 0.905 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? | ?, ?, ? | ?, ?, ? | 0.122, 0.606, 3.25 |
No. of reflections | ? | ? | ? | 2456 |
No. of parameters | ? | ? | ? | 52 |
No. of restraints | 0 | 0 | 0 | 0 |
H-atom treatment | See text | See text | See text | H atoms treated by a mixture of independent and constrained refinement |
| ? | ? | ? | w = 1/[σ2(Fo2) + (0.2P)2] where P = (Fo2 + 2Fc2)/3 |
(Δ/σ)max | ? | ? | ? | 0.551 |
Δρmax, Δρmin (e Å−3) | ?, ? | ?, ? | ?, ? | 1.20, −3.52 |
Absolute structure | ? | ? | ? | ? |
Absolute structure parameter | nne | nne | nne | ? |
| (30) |
Crystal data |
Chemical formula | C6H18Cl2N2Pd |
Mr | 295.54 |
Crystal system, space group | Monclinic, C2/m |
Temperature (K) | 0 |
a, b, c (Å) | 8.929 (2), 8.437 (2), 7.542 (2) |
α, β, γ (°) | 90, 92.65 (3), 90 |
V (Å3) | 567.6 (2) |
Z | 2 |
Radiation type | Mo K\a |
µ (mm−1) | 2.06 |
Crystal size (mm) | × × |
|
Data collection |
Diffractometer | ? |
Absorption correction | – |
No. of measured, independent and observed reflections | ?, ?, ? (?) |
Rint | ? |
Distance from source to specimen (mm) | – |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | ?, ?, ? |
No. of reflections | ? |
No. of parameters | ? |
No. of restraints | 0 |
H-atom treatment | See text |
| ? |
(Δ/σ)max | ? |
Δρmax, Δρmin (e Å−3) | ?, ? |
Absolute structure | ? |
Absolute structure parameter | nne |
Selected geometric parameters (Å, º) for (1) topCu1—O1 | 2.4422 | S1—O2 | 1.492 |
Cu1—O5 | 1.9754 | N1—C1 | 1.3409 |
Cu1—N1 | 2.0023 | N1—C5 | 1.3463 |
S1—O1 | 1.4594 | | |
| | | |
O1—Cu1—O5 | 85.52 | O5i—Cu1—N1i | 93.16 |
O1—Cu1—N1 | 93.09 | O1—S1—O2 | 109.63 |
O1—Cu1—O1i | 176.6 | O1—S1—O1ii | 111.41 |
O1—Cu1—O5i | 92.14 | O1—S1—O2ii | 109.02 |
O1—Cu1—N1i | 89.49 | O1ii—S1—O2 | 109.02 |
O5—Cu1—N1 | 93.16 | O2—S1—O2ii | 108.08 |
O1i—Cu1—O5 | 92.14 | O1ii—S1—O2ii | 109.63 |
O5—Cu1—O5i | 92.94 | Cu1—O1—S1 | 132.63 |
O5—Cu1—N1i | 172.26 | Cu1—N1—C1 | 125.82 |
O1i—Cu1—N1 | 89.49 | Cu1—N1—C5 | 114.86 |
O5i—Cu1—N1 | 172.26 | C1—N1—C5 | 119.32 |
N1—Cu1—N1i | 81.19 | N1—C1—C2 | 122.26 |
O1i—Cu1—O5i | 85.52 | N1—C5—C4 | 121.62 |
O1i—Cu1—N1i | 93.09 | N1—C5—C5i | 114.54 |
Symmetry codes: (i) −x+3/2, y, −z+1; (ii) −x+1/2, y, −z+1. |
Hydrogen-bond geometry (Å, º) for (2) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O14 | 0.91 | 2.52 | 2.8941 | 105 |
N1—H1···O17 | 0.91 | 2.55 | 2.8964 | 103 |
N1—H1···Cl1i | 0.91 | 2.54 | 3.2518 | 136 |
N1—H1···Cl1ii | 0.91 | 2.54 | 3.2518 | 136 |
N4—H6···O14iii | 0.91 | 2.43 | 3.2068 | 143 |
N4—H6···O14iv | 0.91 | 2.43 | 3.2068 | 143 |
N10—H16···Cl1v | 0.91 | 2.3 | 3.137 (2) | 153 |
N10—H16···Cl1vi | 0.91 | 2.3 | 3.137 (2) | 153 |
O19—H21···Cl1vii | 1.2 | 2.51 | 3.290 (3) | 121 |
O19—H21···Cl1viii | 1.2 | 2.51 | 3.290 (3) | 121 |
C2—H2···O17 | 0.97 | 2.6 | 3.1609 | 117 |
C9—H14···O14 | 0.97 | 2.56 | 3.1488 | 119 |
Symmetry codes: (i) −x, −y+1, z+1/2; (ii) x, −y+1, z+1/2; (iii) −x+1, −y+1, z−1/2; (iv) x, −y+1, z−1/2; (v) −x+1/2, −y+1/2, z+1/2; (vi) x+1/2, −y+1/2, z+1/2; (vii) x+1/2, y−1/2, z; (viii) −x+1/2, y−1/2, z. |
Selected geometric parameters (Å, º) for (3) topSi1—O2 | 1.6466 | N1—C1 | 1.328 |
Si1—O4 | 1.6254 | N1—C4 | 1.3573 |
Si1—C19 | 1.8674 | N2—C1 | 1.3394 |
Si1—C22 | 1.8673 | N2—C2 | 1.3451 |
Si2—O3 | 1.6409 | N3—C4 | 1.3455 |
Si2—O4 | 1.6255 | N4—C3 | 1.3851 |
Si2—C13 | 1.8808 | N4—C5 | 1.3192 |
Si2—C16 | 1.86 | N5—C2 | 1.3674 |
O1—C7 | 1.4191 | N5—C5 | 1.3747 |
O2—C8 | 1.4329 | N5—C6 | 1.4712 |
O3—C11 | 1.4277 | | |
| | | |
O2—Si1—O4 | 109.33 | N2—C2—C3 | 125.51 |
O2—Si1—C19 | 105.19 | N5—C2—C3 | 105.75 |
O2—Si1—C22 | 109.05 | N4—C3—C2 | 111.82 |
O4—Si1—C19 | 110.16 | N4—C3—C4 | 130.26 |
O4—Si1—C22 | 107.51 | N1—C4—N3 | 119.21 |
C19—Si1—C22 | 115.49 | N1—C4—C3 | 118.25 |
O3—Si2—O4 | 109.86 | N3—C4—C3 | 122.54 |
O3—Si2—C13 | 108.85 | N4—C5—N5 | 114.81 |
O3—Si2—C16 | 103.33 | N5—C6—C7 | 112.68 |
O4—Si2—C13 | 107.05 | N5—C6—C10 | 111.42 |
O4—Si2—C16 | 111.14 | O1—C7—C6 | 114.74 |
C13—Si2—C16 | 116.49 | O1—C7—C8 | 115.24 |
Si1—O2—C8 | 122.23 | O2—C8—C7 | 112.43 |
Si2—O3—C11 | 123.06 | O2—C8—C9 | 109.95 |
Si1—O4—Si2 | 155.36 | O3—C11—C9 | 110.18 |
C1—N1—C4 | 117.83 | Si2—C13—C12 | 113.36 |
C1—N2—C2 | 111.1 | Si2—C13—C14 | 114.64 |
C3—N4—C5 | 102.29 | Si2—C16—C15 | 113.75 |
C2—N5—C5 | 105.33 | Si2—C16—C17 | 111.63 |
C2—N5—C6 | 129.11 | Si1—C19—C18 | 112.59 |
C5—N5—C6 | 125.53 | Si1—C19—C20 | 111.04 |
N1—C1—N2 | 129.39 | Si1—C22—C21 | 111.28 |
N2—C2—N5 | 128.74 | Si1—C22—C23 | 114.39 |
Selected geometric parameters (Å, º) for (4) topO1—C6 | 1.2242 | | |
| | | |
O1—C6—C1 | 121.59 | O1—C6—C5 | 120.71 |
Selected geometric parameters (Å, º) for (5) topCu1—Cl1 | 2.6316 | N2—C3 | 1.4588 |
Cu1—N1 | 2.0361 | N2—C4 | 1.4975 |
Cu1—N2 | 2.0332 | N3—C5 | 1.4504 |
Cu1—N3 | 2.0616 | N3—C6 | 1.4803 |
Cu1—N4 | 2.0623 | N4—C8 | 1.4992 |
N1—C1 | 1.5045 | N4—C9 | 1.4884 |
| | | |
Cl1—Cu1—N1 | 89.25 | Cu1—N3—C5 | 107.56 |
Cl1—Cu1—N2 | 94.83 | Cu1—N3—C6 | 117.53 |
Cl1—Cu1—N3 | 97.72 | C5—N3—C6 | 111.27 |
Cl1—Cu1—N4 | 94.02 | Cu1—N4—C8 | 114.26 |
N1—Cu1—N2 | 91.72 | Cu1—N4—C9 | 115.4 |
N1—Cu1—N3 | 172.47 | C8—N4—C9 | 109.38 |
N1—Cu1—N4 | 92.02 | N1—C1—C2 | 111.47 |
N2—Cu1—N3 | 84.87 | N2—C3—C2 | 113.32 |
N2—Cu1—N4 | 170.43 | N2—C4—C5 | 108.46 |
N3—Cu1—N4 | 90.35 | N3—C5—C4 | 108.13 |
Cu1—N1—C1 | 122.41 | N3—C6—C7 | 110.69 |
Cu1—N2—C3 | 122.16 | N4—C8—C7 | 114.79 |
Cu1—N2—C4 | 106.51 | N4—C9—C10 | 111.95 |
C3—N2—C4 | 111.36 | | |
Hydrogen-bond geometry (Å, º) for (5) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H3···Cl1i | 0.91 | 2.410 | 3.2535 | 153 |
N3—H4···Cl3 | 0.92 | 2.5 | 3.3713 | 160 |
N4—H5···O1ii | 0.92 | 2.19 | 3.0138 | 149 |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) −x+1, y−1/2, −z+1/2. |
Selected geometric parameters (Å, º) for (6) topCa1—O1 | 2.3783 | O7—C10 | 1.3284 |
Ca1—O4 | 2.2697 | O7—C11 | 1.3518 |
S1—C1 | 1.871 | N1—C2 | 1.4406 |
S1—C3 | 1.8361 | N1—C3 | 1.4595 |
O3—C5 | 1.1817 | N1—C5 | 1.3679 |
O4—C8 | 1.2647 | N2—C4 | 1.4505 |
O5—C8 | 1.2046 | N2—C9 | 1.318 |
O6—C9 | 1.2721 | | |
| | | |
O1—Ca1—O4 | 93.04 | S1—C1—C2 | 101.82 |
O1—Ca1—O1i | 170.13 | S1—C1—C6 | 107.96 |
O1—Ca1—O4i | 93.41 | S1—C1—C7 | 110.04 |
O1—Ca1—O6ii | 88.55 | N1—C2—C1 | 105.13 |
O1—Ca1—O6iii | 83.96 | N1—C2—C8 | 112.06 |
O1i—Ca1—O4 | 93.41 | S1—C3—N1 | 104.65 |
O4—Ca1—O4i | 98.28 | S1—C3—C4 | 117.83 |
O4—Ca1—O6ii | 90.26 | N1—C3—C4 | 87.93 |
O4—Ca1—O6iii | 171.12 | N2—C4—C3 | 117.35 |
O1i—Ca1—O4i | 93.04 | N2—C4—C5 | 112.76 |
O1i—Ca1—O6ii | 83.96 | O3—C5—N1 | 134.13 |
O1i—Ca1—O6iii | 88.55 | O3—C5—C4 | 134.84 |
O4i—Ca1—O6ii | 171.12 | N1—C5—C4 | 90.93 |
O4i—Ca1—O6iii | 90.26 | O4—C8—O5 | 126.36 |
O6ii—Ca1—O6iii | 81.33 | O4—C8—C2 | 115.36 |
C1—S1—C3 | 95.98 | O5—C8—C2 | 118.28 |
Ca1—O4—C8 | 156.36 | O6—C9—N2 | 118.84 |
Ca1iv—O6—C9 | 146.71 | O6—C9—C10 | 124.94 |
C10—O7—C11 | 117.55 | N2—C9—C10 | 116.22 |
C2—N1—C3 | 117.9 | O7—C10—C9 | 114.48 |
C2—N1—C5 | 125.23 | O7—C11—C12 | 116.7 |
C3—N1—C5 | 95.63 | O7—C11—C16 | 123.74 |
C4—N2—C9 | 124.33 | | |
Symmetry codes: (i) x, −y+1, −z; (ii) x+1/2, y−1/2, z; (iii) x+1/2, −y+3/2, −z; (iv) x−1/2, y+1/2, z. |
Selected geometric parameters (Å, º) for (7) topPt—N1 | 2.0252 | N3—C4 | 1.1886 |
Pt—C6 | 1.8186 | N4—C5 | 1.179 |
O1—C6 | 1.1063 | N9—C18 | 1.5651 |
N1—C1 | 1.4106 | N9—C13 | 1.4363 (18) |
N1—C3 | 1.3697 | N9—C17 | 1.5511 (19) |
N2—C1 | 1.4111 | N10—C20 | 1.1330 (14) |
N2—C2 | 1.3153 | | |
| | | |
N1—Pt—C6 | 96.98 | C13—N9—C17 | 120.93 |
N1—Pt—N1i | 79.06 | N2—C1—C1i | 130.84 |
N1—Pt—C6i | 175.95 | N1—C1—N2 | 114.19 |
N1i—Pt—C6 | 175.95 | N1—C1—C1i | 114.96 |
C6—Pt—C6i | 86.96 | N2—C2—C4 | 119.07 |
N1i—Pt—C6i | 96.98 | N2—C2—C3 | 110.79 |
Pt—N1—C1 | 115.46 | N1—C3—C5 | 120.35 |
Pt—N1—C3 | 145.4 | N1—C3—C2 | 113.06 |
C1—N1—C3 | 99.11 | N3—C4—C2 | 176.48 |
C1—N2—C2 | 102.85 | N4—C5—C3 | 176.56 |
C17—N9—C18 | 109.5 | Pt—C6—O1 | 176.03 |
C17—N9—C18ii | 109.5 | N9—C17—C19 | 100.18 |
C18—N9—C18ii | 92.75 | N9—C18—C15 | 96.54 |
C13—N9—C18 | 110.26 | N10—C20—C21 | 178.26 |
C13—N9—C18ii | 110.26 | | |
Symmetry codes: (i) −x+1, y, z; (ii) −x, y, z. |
Selected geometric parameters (Å, º) for (8) topCl1—C1 | 1.7422 (4) | O3—C11 | 1.3830 (3) |
O1—C4 | 1.3566 (3) | O3—C12 | 1.3875 (3) |
O1—C7 | 1.4229 (3) | O4—C11 | 1.1898 (3) |
O2—C5 | 1.3490 (3) | N1—C10 | 1.4098 (3) |
O2—C8 | 1.4382 (3) | N1—C12 | 1.2702 (3) |
| | | |
C4—O1—C7 | 116.3 | O2—C5—C6 | 125.11 |
C5—O2—C8 | 117.31 | N1—C10—C9 | 130.35 |
C11—O3—C12 | 105.62 | N1—C10—C11 | 107.64 |
C10—N1—C12 | 105.6 | O3—C11—O4 | 121.84 |
Cl1—C1—C2 | 120.56 | O3—C11—C10 | 104.8 |
Cl1—C1—C6 | 116.71 | O4—C11—C10 | 133.36 |
O1—C4—C3 | 125.23 | O3—C12—N1 | 116.33 |
O1—C4—C5 | 114.61 | O3—C12—C13 | 115.15 |
O2—C5—C4 | 115.71 | N1—C12—C13 | 128.51 |
Selected geometric parameters (Å, º) for (9) topP1—O1 | 1.5127 | O25—O28 | 1.0792 |
P1—O2 | 1.626 | N1—C6 | 1.3411 |
P1—O3 | 1.5083 | N1—C8 | 1.36 |
P1—O4 | 1.4939 | N1—C3 | 1.4923 |
O2—C1 | 1.4252 | N2—C6 | 1.3474 |
O5—C2 | 1.4569 | N2—C7 | 1.3534 |
O5—C3 | 1.3876 | N3—C9 | 1.3018 |
O6—C4 | 1.4129 | N3—C8 | 1.336 |
O7—C5 | 1.4082 | N4—C9 | 1.3519 |
O8—C10 | 1.2095 | N4—C10 | 1.3772 |
| | | |
O1—P1—O2 | 106.42 | O5—C3—N1 | 107.61 |
O1—P1—O3 | 112.19 | O5—C3—C4 | 106.19 |
O1—P1—O4 | 111.94 | N1—C3—C4 | 113.27 |
O2—P1—O3 | 103.7 | O6—C4—C3 | 108.83 |
O2—P1—O4 | 107.17 | O6—C4—C5 | 114.64 |
O3—P1—O4 | 114.6 | O7—C5—C2 | 109.64 |
P1—O2—C1 | 115.03 | O7—C5—C4 | 106.39 |
C2—O5—C3 | 109.72 | N1—C6—N2 | 111.48 |
C3—N1—C6 | 126.62 | N2—C7—C8 | 112.02 |
C3—N1—C8 | 124.4 | N2—C7—C10 | 130.1 |
C6—N1—C8 | 108.76 | N1—C8—N3 | 127.95 |
C6—N2—C7 | 103.82 | N1—C8—C7 | 103.81 |
C8—N3—C9 | 111.98 | N3—C8—C7 | 128.18 |
C9—N4—C10 | 124.78 | N3—C9—N4 | 125.58 |
O2—C1—C2 | 111.67 | O8—C10—N4 | 120.28 |
O5—C2—C1 | 110.65 | O8—C10—C7 | 128.41 |
O5—C2—C5 | 105.67 | N4—C10—C7 | 111.31 |
Selected geometric parameters (Å, º) for (10) topZn3—O1 | 2.0331 | O2—C1 | 1.2431 |
Zn3—O2 | 2.4237 | O3—C3 | 1.2156 |
Zn3—O5 | 1.975 | O4—C3 | 1.2391 |
Zn3—O7 | 1.9819 | O5—C5 | 1.2547 |
Zn3—N1 | 2.06 | O6—C5 | 1.2476 |
Zn4—O3 | 2.114 | O7—C7 | 1.248 |
Zn4—O4 | 2.2458 | O8—C7 | 1.2494 |
Zn4—O6 | 1.9921 | N1—C9 | 1.3485 |
Zn4—N2 | 2.0618 | N1—C13 | 1.3474 |
Zn4—O8i | 1.9982 | N2—C14 | 1.3407 |
O1—C1 | 1.2532 | N2—C18 | 1.337 |
| | | |
O1—Zn3—O2 | 57.01 | Zn4—O6—C5 | 138.98 |
O1—Zn3—O5 | 131.7 | Zn3—O7—C7 | 137.91 |
O1—Zn3—O7 | 121 | Zn4ii—O8—C7 | 111.26 |
O1—Zn3—N1 | 94.27 | Zn3—N1—C9 | 124.09 |
O2—Zn3—O5 | 94.62 | Zn3—N1—C13 | 118.4 |
O2—Zn3—O7 | 101.73 | C9—N1—C13 | 117.42 |
O2—Zn3—N1 | 150.86 | Zn4—N2—C14 | 120.61 |
O5—Zn3—O7 | 101.23 | Zn4—N2—C18 | 121.88 |
O5—Zn3—N1 | 102.9 | C14—N2—C18 | 117.51 |
O7—Zn3—N1 | 97.5 | O1—C1—O2 | 119.31 |
O3—Zn4—O4 | 57.52 | O1—C1—C2 | 117.38 |
O3—Zn4—O6 | 119.64 | O2—C1—C2 | 123.28 |
O3—Zn4—N2 | 94.19 | O3—C3—O4 | 117.72 |
O3—Zn4—O8i | 138.2 | O3—C3—C4 | 121.64 |
O4—Zn4—O6 | 106.57 | O4—C3—C4 | 120.63 |
O4—Zn4—N2 | 149.92 | O5—C5—O6 | 122.09 |
O4—Zn4—O8i | 97.17 | O5—C5—C6 | 117.38 |
O6—Zn4—N2 | 96.07 | O6—C5—C6 | 120.53 |
O6—Zn4—O8i | 98.26 | O7—C7—O8 | 121.87 |
O8i—Zn4—N2 | 98.92 | O7—C7—C8 | 120.01 |
Zn3—O1—C1 | 100.49 | O8—C7—C8 | 118.1 |
Zn3—O2—C1 | 82.49 | N1—C9—C10 | 122.19 |
Zn4—O3—C3 | 95.48 | N1—C13—C12 | 122.42 |
Zn4—O4—C3 | 88.54 | N2—C14—C15 | 122.7 |
Zn3—O5—C5 | 115.97 | N2—C18—C17 | 123.84 |
Symmetry codes: (i) x, y, z−1; (ii) x, y, z+1. |
Selected geometric parameters (Å, º) for (11) topFe1—O1 | 2.1216 | O3—C6 | 1.2337 |
Fe1—N1 | 2.2127 (5) | N1—C1 | 1.3244 |
Fe1—N1i | 2.2127 (5) | | |
| | | |
O1—Fe1—N1 | 92.76 | O1i—Fe1—O1iii | 180 |
O1—Fe1—O1i | 89.69 | O1ii—Fe1—N1i | 92.76 |
O1—Fe1—N1i | 87.24 | O1iii—Fe1—N1i | 87.24 |
O1—Fe1—O1ii | 180 | O1ii—Fe1—O1iii | 89.69 |
O1—Fe1—O1iii | 90.31 | Fe1—N1—C1 | 121.78 |
O1i—Fe1—N1 | 87.24 | Fe1—N1—C1iii | 121.78 |
N1—Fe1—N1i | 180 | C1—N1—C1iii | 116.27 |
O1ii—Fe1—N1 | 87.24 | N1—C1—C2 | 123.69 |
O1iii—Fe1—N1 | 92.76 | O3—C6—C7 | 116.7 |
O1i—Fe1—N1i | 92.76 | O3—C6—O3iii | 126.6 |
O1i—Fe1—O1ii | 90.31 | O3iii—C6—C7 | 116.7 |
Symmetry codes: (i) −x, y, −z+2; (ii) −x, −y, −z+2; (iii) x, −y, z. |
Selected geometric parameters (Å, º) for (13) topFe1—O1 | 2.0382 | O9—C11 | 1.2792 |
Fe1—O3 | 1.9951 | O10—C1 | 1.268 |
Fe1—O4 | 2.007 | N1—C1 | 1.3585 |
Fe1—O7 | 2.0957 | N1—C2 | 1.5151 |
Fe1—O9 | 2.1661 | N1—C4 | 1.4619 |
Fe3—O7 | 2.2104 | N2—C6 | 1.3236 |
Fe3—O9 | 2.0941 | N2—C7 | 1.4862 |
Fe3—O10 | 2.0505 | N2—C8 | 1.4558 |
O1—C26 | 1.2601 | N3—C11 | 1.3448 (2) |
O3—C1 | 1.2736 | N3—C12 | 1.4502 |
O4—C6 | 1.2514 | N6—C26 | 1.3527 (2) |
O7—C6i | 1.3041 | N6—C27 | 1.4456 |
| | | |
O1—Fe1—O3 | 104.67 | Fe3—O9—C11 | 131.54 |
O1—Fe1—O4 | 90.65 | Fe3—O10—C1 | 131.91 |
O1—Fe1—O7 | 92.22 | C1—N1—C2 | 120.87 |
O1—Fe1—O9 | 164.07 | C1—N1—C4 | 120.55 |
O3—Fe1—O4 | 123.4 | C2—N1—C4 | 118.54 |
O3—Fe1—O7 | 93.89 | C6—N2—C7 | 118.91 |
O3—Fe1—O9 | 90.05 | C6—N2—C8 | 123.09 |
O4—Fe1—O7 | 140.41 | C7—N2—C8 | 117.91 |
O4—Fe1—O9 | 86.14 | C11—N3—C12 | 121.3 |
O7—Fe1—O9 | 80.53 | C11—N3—C12iii | 121.3 |
O7—Fe3—O9 | 79.54 | C12—N3—C12iii | 117.4 |
O7—Fe3—O10 | 88.68 | C26—N6—C27 | 120.7 |
O7—Fe3—O7ii | 158.34 | C26—N6—C27i | 120.7 |
O7—Fe3—O9ii | 86.79 | C27—N6—C27i | 118.59 |
O7—Fe3—O10ii | 107.57 | O3—C1—O10 | 126.52 |
O9—Fe3—O10 | 87.56 | O3—C1—N1 | 116.8 |
O7ii—Fe3—O9 | 86.79 | O10—C1—N1 | 116.67 |
O9—Fe3—O9ii | 101.57 | N1—C2—C3 | 107.48 |
O9—Fe3—O10ii | 168.89 | N1—C4—C5 | 108.79 |
O7ii—Fe3—O10 | 107.57 | O4—C6—N2 | 120.09 |
O9ii—Fe3—O10 | 168.89 | O4—C6—O7i | 122.27 |
O10—Fe3—O10ii | 84.14 | O7i—C6—N2 | 117.64 |
O7ii—Fe3—O9ii | 79.54 | N2—C7—C10 | 113.17 |
O7ii—Fe3—O10ii | 88.68 | N2—C8—C9 | 112 |
O9ii—Fe3—O10ii | 87.56 | O9—C11—N3 | 119.42 |
Fe1—O1—C26 | 128.91 | O9—C11—O9iii | 121.17 |
Fe1—O3—C1 | 127.82 | O9iii—C11—N3 | 119.42 |
Fe1—O4—C6 | 123.32 | N3—C12—C13 | 114.23 |
Fe1—O7—Fe3 | 95.71 | O1—C26—N6 | 116.98 |
Fe1—O7—C6i | 124.17 | O1—C26—O1i | 126.05 |
Fe3—O7—C6i | 138.11 | O1i—C26—N6 | 116.98 |
Fe1—O9—Fe3 | 97.11 | N6—C27—C28 | 110.83 |
Fe1—O9—C11 | 128.84 | | |
Symmetry codes: (i) x, −y+1/2, −z+1/2; (ii) −x, y, −z+1/2; (iii) −x, −y+1/2, z. |
Selected geometric parameters (Å, º) for (14) topPd1—P1 | 2.3875 | P1—C15 | 1.8583 |
Pd1—P2 | 2.4038 | P2—C34 | 1.8599 |
P1—C1 | 1.8427 | P2—C35 | 1.8464 |
P1—C8 | 1.8462 | P2—C42 | 1.8512 |
| | | |
P1—Pd1—P2 | 90.85 | C34—P2—C35 | 104.37 |
P1—Pd1—P1i | 122.79 | C34—P2—C42 | 99.68 |
P1—Pd1—P2i | 117.49 | C35—P2—C42 | 100.53 |
P1i—Pd1—P2 | 117.49 | P1—C1—C2 | 117.38 |
P2—Pd1—P2i | 120.33 | P1—C1—C6 | 125.16 |
P1i—Pd1—P2i | 90.85 | P1—C8—C9 | 119.87 |
Pd1—P1—C1 | 115.41 | P1—C8—C13 | 122.44 |
Pd1—P1—C8 | 122.62 | P1—C15—C16 | 116.78 |
Pd1—P1—C15 | 111.31 | P1—C15—C24 | 123.52 |
C1—P1—C8 | 100.53 | P2—C34—C25 | 124.57 |
C1—P1—C15 | 105.96 | P2—C34—C33 | 117.11 |
C8—P1—C15 | 98.68 | P2—C35—C36 | 117.31 |
Pd1—P2—C34 | 111.13 | P2—C35—C40 | 125.56 |
Pd1—P2—C35 | 116.89 | P2—C42—C43 | 118.07 |
Pd1—P2—C42 | 121.68 | P2—C42—C47 | 126.31 |
Symmetry code: (i) −x, y, −z+1/2. |
Selected geometric parameters (Å, º) for (16) topCd1—O1 | 2.3439 | O1—C1 | 1.2619 |
Cd1—O2 | 2.4162 | O2—C1 | 1.2631 |
Cd1—O5 | 2.2901 (3) | N1—C5 | 1.4151 |
Cd1—C1 | 2.7365 | | |
| | | |
O1—Cd1—O2 | 54.72 | N1ii—Cd1—C1 | 89.26 |
O1—Cd1—O5 | 82.86 | N1iii—Cd1—C1 | 94.23 |
O1—Cd1—C1 | 27.39 | O1i—Cd1—O2i | 54.72 |
O1—Cd1—O1i | 165.73 | O1i—Cd1—C1i | 27.39 |
O1—Cd1—O2i | 139.51 | O1i—Cd1—N1ii | 87.88 |
O1—Cd1—C1i | 166.57 | O1i—Cd1—N1iii | 90.85 |
O1—Cd1—N1ii | 90.85 | O2i—Cd1—C1i | 27.49 |
O1—Cd1—N1iii | 87.88 | O2i—Cd1—N1ii | 95.84 |
O2—Cd1—O5 | 137.43 | O2i—Cd1—N1iii | 91.69 |
O2—Cd1—C1 | 27.49 | N1ii—Cd1—C1i | 94.23 |
O1i—Cd1—O2 | 139.51 | N1iii—Cd1—C1i | 89.26 |
O2—Cd1—O2i | 85.13 | N1ii—Cd1—N1iii | 169.78 |
O2—Cd1—C1i | 112.62 | Cd1—O1—C1 | 93.9 |
O2—Cd1—N1ii | 91.69 | Cd1—O2—C1 | 90.51 |
O2—Cd1—N1iii | 95.84 | Cd1ii—N1—C5 | 114.28 |
O5—Cd1—C1 | 109.95 | Cd1—C1—O1 | 58.71 |
O1i—Cd1—O5 | 82.86 | Cd1—C1—O2 | 62 |
O2i—Cd1—O5 | 137.43 | Cd1—C1—C2 | 169.59 |
O5—Cd1—C1i | 109.95 | O1—C1—O2 | 120.17 |
O5—Cd1—N1ii | 84.89 | O1—C1—C2 | 119.65 |
O5—Cd1—N1iii | 84.89 | O2—C1—C2 | 120.09 |
O1i—Cd1—C1 | 166.57 | N1—C5—C4 | 120.24 |
O2i—Cd1—C1 | 112.62 | N1—C5—C6 | 120.41 |
C1—Cd1—C1i | 140.1 | | |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, −y, −z; (iii) x, −y, z+1/2. |
Selected geometric parameters (Å, º) for (17) topFe1—C1 | 2.0531 | Fe1—C9 | 2.0326 |
Fe1—C2 | 2.0468 | Fe1—C10 | 2.0394 |
Fe1—C3 | 2.0336 | O1—C13 | 1.1936 |
Fe1—C4 | 2.0216 | O2—C13 | 1.3941 |
Fe1—C5 | 2.0210 | O2—C14 | 1.3901 |
Fe1—C6 | 2.0308 | N1—C12 | 1.3944 |
Fe1—C7 | 2.0341 | N1—C14 | 1.2817 |
Fe1—C8 | 2.0378 | | |
| | | |
C1—Fe1—C2 | 40.72 | C6—Fe1—C10 | 40.22 |
C1—Fe1—C3 | 68.37 | C7—Fe1—C8 | 40.49 |
C1—Fe1—C4 | 68.58 | C7—Fe1—C9 | 68.14 |
C1—Fe1—C5 | 41.23 | C7—Fe1—C10 | 67.9 |
C1—Fe1—C6 | 124.33 | C8—Fe1—C9 | 40.57 |
C1—Fe1—C7 | 157.54 | C8—Fe1—C10 | 67.9 |
C1—Fe1—C8 | 161.78 | C9—Fe1—C10 | 40.32 |
C1—Fe1—C9 | 127.13 | C13—O2—C14 | 105.52 |
C1—Fe1—C10 | 111.65 | C12—N1—C14 | 105.97 |
C2—Fe1—C3 | 40.61 | Fe1—C1—C2 | 69.4 |
C2—Fe1—C4 | 68.37 | Fe1—C1—C5 | 68.19 |
C2—Fe1—C5 | 68.94 | Fe1—C1—C11 | 125 |
C2—Fe1—C6 | 109.72 | Fe1—C2—C1 | 69.88 |
C2—Fe1—C7 | 120.59 | Fe1—C2—C3 | 69.19 |
C2—Fe1—C8 | 153.96 | Fe1—C3—C2 | 70.2 |
C2—Fe1—C9 | 164.75 | Fe1—C3—C4 | 69.33 |
C2—Fe1—C10 | 128.23 | Fe1—C4—C3 | 70.25 |
C3—Fe1—C4 | 40.42 | Fe1—C4—C5 | 69.62 |
C3—Fe1—C5 | 68.52 | Fe1—C5—C1 | 70.59 |
C3—Fe1—C6 | 124.71 | Fe1—C5—C4 | 69.66 |
C3—Fe1—C7 | 105.28 | Fe1—C6—C7 | 69.88 |
C3—Fe1—C8 | 117.74 | Fe1—C6—C10 | 70.22 |
C3—Fe1—C9 | 153.42 | Fe1—C7—C6 | 69.63 |
C3—Fe1—C10 | 163.03 | Fe1—C7—C8 | 69.9 |
C4—Fe1—C5 | 40.72 | Fe1—C8—C7 | 69.62 |
C4—Fe1—C6 | 159.36 | Fe1—C8—C9 | 69.52 |
C4—Fe1—C7 | 121.39 | Fe1—C9—C8 | 69.91 |
C4—Fe1—C8 | 104.26 | Fe1—C9—C10 | 70.1 |
C4—Fe1—C9 | 119.45 | Fe1—C10—C6 | 69.56 |
C4—Fe1—C10 | 156.47 | Fe1—C10—C9 | 69.58 |
C5—Fe1—C6 | 159.46 | N1—C12—C11 | 127.9 |
C5—Fe1—C7 | 158.47 | N1—C12—C13 | 108.45 |
C5—Fe1—C8 | 122.62 | O1—C13—O2 | 121.45 |
C5—Fe1—C9 | 107.68 | O1—C13—C12 | 133.91 |
C5—Fe1—C10 | 123.5 | O2—C13—C12 | 104.63 |
C6—Fe1—C7 | 40.49 | O2—C14—N1 | 115.41 |
C6—Fe1—C8 | 67.99 | O2—C14—C15 | 116.61 |
C6—Fe1—C9 | 67.9 | N1—C14—C15 | 127.97 |
Selected geometric parameters (Å, º) for (18) topCl1—Mg1 | 2.4772 (6) | Mg1—O3 | 2.1063 (5) |
Mg2—O6 | 2.077 | Mg1—O4 | 2.1003 (5) |
Mg2—O5i | 2.0415 (5) | O6—C6 | 1.2245 |
Mg2—O5 | 2.0415 (5) | O3—C1 | 1.2011 (3) |
Mg1—O1 | 2.0384 | O4—C3 | 1.2221 (3) |
| | | |
O5—Mg2—O6 | 90.51 | O1—Mg1—O3 | 84.8 |
O5—Mg2—O5i | 180 | O1—Mg1—O4 | 86.08 |
O5—Mg2—O6i | 89.49 | O1—Mg1—O1iv | 167.72 |
O5—Mg2—O6ii | 89.49 | Cl1—Mg1—O1 | 95.18 |
O5—Mg2—O6iii | 90.51 | Cl1—Mg1—O3 | 179.57 |
O5i—Mg2—O6 | 89.49 | O1iv—Mg1—O4 | 86.08 |
O6—Mg2—O6i | 83.15 | O3—Mg1—O4 | 82.4 |
O6—Mg2—O6ii | 180 | O1iv—Mg1—O3 | 84.8 |
O6—Mg2—O6iii | 96.85 | Mg2—O6—C6 | 133.43 |
O5i—Mg2—O6i | 90.51 | Mg1—O3—C1 | 134.12 |
O5i—Mg2—O6ii | 90.51 | Mg1—O4—C3 | 133.33 |
O5i—Mg2—O6iii | 89.49 | O6—C6—C9 | 119.28 |
O6i—Mg2—O6ii | 96.85 | O6—C6—C7 | 123.81 |
O6i—Mg2—O6iii | 180 | O3—C1—C2 | 124.29 |
O6ii—Mg2—O6iii | 83.15 | O3—C1—C4 | 121.82 |
Cl1—Mg1—O4 | 97.16 | O4—C3—C2 | 125.18 |
Cl1—Mg1—O1iv | 95.18 | O4—C3—C5 | 121.65 |
Symmetry codes: (i) x, −y+1, −z; (ii) −x+1, −y+1, −z; (iii) −x+1, y, z; (iv) −x, y, z. |
Selected geometric parameters (Å, º) for (19) topRe1—N1 | 2.2428 | O1—C1 | 1.1158 |
Re1—N3 | 2.1002 | O2—C2 | 1.1837 |
Re1—C1 | 2.0112 | O3—C3 | 1.1025 |
Re1—C2 | 1.9589 | O4—C4 | 1.1653 |
Re1—C3 | 1.9629 | O5—C5 | 1.1840 (5) |
Re1—C4 | 1.9251 | O6—C6 | 1.1824 |
Re2—N13 | 2.1048 | O7—C7 | 1.0892 (5) |
Re2—C5 | 1.9908 (9) | N1—N13 | 1.0394 |
Re2—C6 | 1.9136 | N3—N3i | 1.166 |
Re2—C7 | 2.0321 (9) | | |
| | | |
N1—Re1—N3 | 83.63 | C5—Re2—C6 | 90.52 |
N1—Re1—C1 | 89.37 | C5—Re2—C7 | 179.97 |
N1—Re1—C2 | 88.63 | N13i—Re2—C5 | 86.84 |
N1—Re1—C3 | 176.62 | C5—Re2—C6i | 90.52 |
N1—Re1—C4 | 90.27 | C6—Re2—C7 | 89.49 |
N3—Re1—C1 | 82.5 | N13i—Re2—C6 | 170.86 |
N3—Re1—C2 | 94.2 | C6—Re2—C6i | 94.92 |
N3—Re1—C3 | 93.15 | N13i—Re2—C7 | 93.15 |
N3—Re1—C4 | 171.75 | C6i—Re2—C7 | 89.49 |
C1—Re1—C2 | 176.32 | N13i—Re2—C6i | 93.85 |
C1—Re1—C3 | 91.23 | Re1—N1—N13 | 162.55 |
C1—Re1—C4 | 91.91 | Re1—N3—N3i | 165.84 |
C2—Re1—C3 | 90.58 | Re2—N13—N1 | 174.98 |
C2—Re1—C4 | 91.2 | Re1—C1—O1 | 176.52 |
C3—Re1—C4 | 93.03 | Re1—C2—O2 | 173.86 |
N13—Re2—C5 | 86.84 | Re1—C3—O3 | 175.66 |
N13—Re2—C6 | 93.85 | Re1—C4—O4 | 175.06 |
N13—Re2—C7 | 93.15 | Re2—C5—O5 | 178.51 |
N13—Re2—N13i | 77.28 | Re2—C6—O6 | 177.85 |
N13—Re2—C6i | 170.86 | Re2—C7—O7 | 175.09 |
Symmetry code: (i) x, −y+1/2, z. |
Selected geometric parameters (Å, º) for (20) topS1—C1 | 1.7507 (5) | N1—N2 | 1.3892 (4) |
S1—C4 | 1.7818 (5) | N1—C1 | 1.2808 (4) |
S2—C1 | 1.7193 (5) | N2—C2 | 1.2948 (4) |
S2—C2 | 1.7216 (5) | N3—C10 | 1.1434 (3) |
| | | |
C1—S1—C4 | 101.60 (6) | S2—C2—N2 | 113.67 (6) |
C1—S2—C2 | 86.74 (6) | S2—C2—C3 | 122.61 (6) |
N2—N1—C1 | 111.55 (6) | N2—C2—C3 | 123.72 (6) |
N1—N2—C2 | 112.87 (6) | S1—C4—C5 | 119.51 |
S1—C1—S2 | 125.95 (6) | S1—C4—C5i | 119.51 |
S1—C1—N1 | 118.89 (6) | N3—C10—C7 | 178.92 (6) |
S2—C1—N1 | 115.16 (6) | | |
Symmetry code: (i) x, −y+1/2, z. |
Hydrogen-bond geometry (Å, º) for (20) top
D—H···A | D—H | H···A | D···A | D—H···A |
C3—H1···N1ii | 0.96 | 2.31 | 3.2331 (9) | 162 |
C3—H1···N2ii | 0.96 | 2.48 | 3.4204 (9) | 165 |
C3—H1···N1iii | 0.96 | 2.31 | 3.2331 (9) | 162 |
C3—H1···N2iii | 0.96 | 2.48 | 3.4204 (9) | 165 |
Symmetry codes: (ii) x+1, y, z; (iii) x+1, −y+1/2, z. |
Selected geometric parameters (Å, º) for (21) topPt1—Cl1 | 2.2841 (13) | Pt1—Cl1i | 2.3924 (14) |
Pt1—Cl2 | 2.1232 (12) | O1—C1 | 1.0741 (6) |
Pt1—C1 | 1.8520 (11) | | |
| | | |
Cl1—Pt1—Cl2 | 93.96 | Cl1i—Pt1—Cl2 | 179.26 |
Cl1—Pt1—C1 | 176.63 | Cl1i—Pt1—C1 | 91.34 |
Cl1—Pt1—Cl1i | 85.29 | Pt1—Cl1—Pt1i | 94.71 |
Cl2—Pt1—C1 | 89.41 | Pt1—C1—O1 | 179.7 |
Symmetry code: (i) −x+1, −y, z. |
Selected geometric parameters (Å, º) for (22) topO1—C3 | 1.1986 (7) | N1—C4 | 1.3747 (8) |
O2—C4 | 1.1957 (7) | N1—C7 | 1.4998 |
N1—C3 | 1.3680 (8) | N1—C7' | 1.4998 |
| | | |
C3—N1—C4 | 134.29 (4) | O2—C4—C5 | 128.66 (4) |
C3—N1—C7 | 112.78 | N1—C7—C1 | 101.01 |
C3—N1—C7' | 112.78 | N1—C7—C1' | 103.38 |
C4—N1—C7 | 112.02 | N1—C7—C6 | 100.78 |
C4—N1—C7' | 112.02 | N1—C7—C6' | 103.85 |
C7—N1—C7' | 22.26 | N1—C7—C7' | 78.87 |
O1—C3—N1 | 125.73 (4) | N1—C7'—C1 | 103.38 |
O1—C3—C2 | 128.06 (4) | N1—C7'—C1' | 101.01 |
N1—C3—C2 | 106.21 (4) | N1—C7'—C6 | 103.85 |
O2—C4—N1 | 125.17 (4) | N1—C7'—C6' | 100.78 |
N1—C4—C5 | 106.17 (4) | N1—C7'—C7 | 78.87 |
Selected geometric parameters (Å, º) for (23) topRe1—Cl1 | 2.4227 | S2—C2 | 1.8353 |
Re1—S1 | 2.4012 | P1—C4 | 1.8363 |
Re1—P1 | 2.4815 | P1—C10 | 1.8258 |
Re1—N1 | 1.8064 | P1—C16 | 1.8399 |
S1—C1 | 1.6891 | N1—N3 | 1.238 |
S2—C1 | 1.7425 | N3—C1 | 1.3643 |
| | | |
Cl1—Re1—S1 | 174.15 | Re1—P1—C4 | 115.22 |
Cl1—Re1—P1 | 84.2 | Re1—P1—C10 | 113.4 |
Cl1—Re1—N1 | 100.76 | Re1—P1—C16 | 115.46 |
Cl1—Re1—Cl1i | 75.26 | C4—P1—C10 | 104.53 |
Cl1—Re1—S1i | 110.42 | C4—P1—C16 | 104.22 |
Cl1—Re1—P1i | 88.28 | C10—P1—C16 | 102.57 |
Cl1—Re1—N1i | 175.97 | Re1—N1—N3 | 140.04 |
S1—Re1—P1 | 97.2 | N1—N3—C1 | 112.22 |
S1—Re1—N1 | 73.58 | S1—C1—S2 | 121.84 |
Cl1i—Re1—S1 | 110.42 | S1—C1—N3 | 114.38 |
S1—Re1—S1i | 63.95 | S1—C1—S1i | 97.67 |
S1—Re1—P1i | 90.86 | S1—C1—S2i | 139.73 |
S1—Re1—N1i | 9.68 | S1—C1—N3i | 16.88 |
P1—Re1—N1 | 90.68 | S2—C1—N3 | 122.86 |
Cl1i—Re1—P1 | 88.28 | S1i—C1—S2 | 139.73 |
S1i—Re1—P1 | 90.86 | S2—C1—S2i | 22.8 |
P1—Re1—P1i | 170.51 | S2—C1—N3i | 105.53 |
P1—Re1—N1i | 96.42 | S1i—C1—N3 | 16.88 |
Cl1i—Re1—N1 | 175.97 | S2i—C1—N3 | 105.53 |
S1i—Re1—N1 | 9.68 | N3—C1—N3i | 131.18 |
P1i—Re1—N1 | 96.42 | S1i—C1—S2i | 121.84 |
N1—Re1—N1i | 83.22 | S1i—C1—N3i | 114.38 |
Cl1i—Re1—S1i | 174.15 | S2i—C1—N3i | 122.86 |
Cl1i—Re1—P1i | 84.2 | P1—C4—C5 | 122.33 |
Cl1i—Re1—N1i | 100.76 | P1—C4—C9 | 118.22 |
S1i—Re1—P1i | 97.2 | P1—C10—C11 | 122.55 |
S1i—Re1—N1i | 73.58 | P1—C10—C15 | 117.34 |
P1i—Re1—N1i | 90.68 | P1—C16—C17 | 118.65 |
Re1—S1—C1 | 99.19 | P1—C16—C21 | 121.37 |
C1—S2—C2 | 106.21 | | |
Symmetry code: (i) −x+1, y, −z+1/2. |
Selected geometric parameters (Å, º) for (25) topCr1—C1 | 2.1423 | Cr1—C4 | 2.1315 |
Cr1—C3 | 2.133 | | |
| | | |
C1—Cr1—C3 | 38.11 | C1i—Cr1—C3iii | 141.89 |
C1—Cr1—C4 | 69.77 | C1i—Cr1—C4iii | 110.23 |
C1—Cr1—C1i | 141.63 | C3i—Cr1—C4i | 38.61 |
C1—Cr1—C3i | 110.96 | C1ii—Cr1—C3i | 69.04 |
C1—Cr1—C4i | 97.37 | C3i—Cr1—C3ii | 81.56 |
C1—Cr1—C1ii | 180 | C3i—Cr1—C4ii | 69.57 |
C1—Cr1—C3ii | 141.89 | C1iii—Cr1—C3i | 141.89 |
C1—Cr1—C4ii | 110.23 | C3i—Cr1—C3iii | 180 |
C1—Cr1—C1iii | 38.37 | C3i—Cr1—C4iii | 141.39 |
C1—Cr1—C3iii | 69.04 | C1ii—Cr1—C4i | 82.63 |
C1—Cr1—C4iii | 82.63 | C3ii—Cr1—C4i | 69.57 |
C3—Cr1—C4 | 38.61 | C4i—Cr1—C4ii | 38.66 |
C1i—Cr1—C3 | 110.96 | C1iii—Cr1—C4i | 110.23 |
C3—Cr1—C3i | 98.44 | C3iii—Cr1—C4i | 141.39 |
C3—Cr1—C4i | 110.43 | C4i—Cr1—C4iii | 180 |
C1ii—Cr1—C3 | 141.89 | C1ii—Cr1—C3ii | 38.11 |
C3—Cr1—C3ii | 180 | C1ii—Cr1—C4ii | 69.77 |
C3—Cr1—C4ii | 141.39 | C1ii—Cr1—C1iii | 141.63 |
C1iii—Cr1—C3 | 69.04 | C1ii—Cr1—C3iii | 110.96 |
C3—Cr1—C3iii | 81.56 | C1ii—Cr1—C4iii | 97.37 |
C3—Cr1—C4iii | 69.57 | C3ii—Cr1—C4ii | 38.61 |
C1i—Cr1—C4 | 97.37 | C1iii—Cr1—C3ii | 110.96 |
C3i—Cr1—C4 | 110.43 | C3ii—Cr1—C3iii | 98.44 |
C4—Cr1—C4i | 141.34 | C3ii—Cr1—C4iii | 110.43 |
C1ii—Cr1—C4 | 110.23 | C1iii—Cr1—C4ii | 97.37 |
C3ii—Cr1—C4 | 141.39 | C3iii—Cr1—C4ii | 110.43 |
C4—Cr1—C4ii | 180 | C4ii—Cr1—C4iii | 141.34 |
C1iii—Cr1—C4 | 82.63 | C1iii—Cr1—C3iii | 38.11 |
C3iii—Cr1—C4 | 69.57 | C1iii—Cr1—C4iii | 69.77 |
C4—Cr1—C4iii | 38.66 | C3iii—Cr1—C4iii | 38.61 |
C1i—Cr1—C3i | 38.11 | Cr1—C1—C3 | 70.59 |
C1i—Cr1—C4i | 69.77 | Cr1—C1—C1iii | 70.82 |
C1i—Cr1—C1ii | 38.37 | Cr1—C3—C1 | 71.31 |
C1i—Cr1—C3ii | 69.04 | Cr1—C3—C4 | 70.64 |
C1i—Cr1—C4ii | 82.63 | Cr1—C4—C3 | 70.75 |
C1i—Cr1—C1iii | 180 | Cr1—C4—C4iii | 70.67 |
Symmetry codes: (i) x, −y, −z; (ii) −x, −y, −z; (iii) −x, y, z. |
Selected geometric parameters (Å, º) for (26) topRe1—Cl1 | 2.4132 (3) | Re1—P1i | 2.4327 (3) |
Re1—Cl3 | 2.4313 (3) | P1—C7 | 1.8002 (2) |
Re1—P1 | 2.4327 (3) | P1—C8 | 1.8168 |
Re1—N1 | 1.6949 (2) | N1—C1 | 1.3998 (2) |
Re1—Cl1i | 2.4132 (3) | | |
| | | |
Cl1—Re1—Cl3 | 87.22 | Cl1i—Re1—N1 | 92.78 |
Cl1—Re1—P1 | 89.66 | P1i—Re1—N1 | 97.03 |
Cl1—Re1—N1 | 92.78 | Cl1i—Re1—P1i | 89.66 |
Cl1—Re1—Cl1i | 174.45 | Re1—P1—C7 | 111.35 |
Cl1—Re1—P1i | 89.66 | Re1—P1—C8 | 116.04 |
Cl3—Re1—P1 | 82.97 | Re1—P1—C8ii | 116.04 |
Cl3—Re1—N1 | 180 | C7—P1—C8 | 104.63 |
Cl1i—Re1—Cl3 | 87.22 | C7—P1—C8ii | 104.63 |
Cl3—Re1—P1i | 82.97 | C8—P1—C8ii | 102.86 |
P1—Re1—N1 | 97.03 | Re1—N1—C1 | 180 |
Cl1i—Re1—P1 | 89.66 | N1—C1—C2 | 120.33 |
P1—Re1—P1i | 165.95 | N1—C1—C2i | 120.33 |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+1, y, z. |
Selected geometric parameters (Å, º) for (27) topIr1—C2 | 2.0839 | Ir2—C2 | 2.3616 |
Ir1—C5 | 2.1905 | Ir2—C1i | 2.2984 |
Ir1—C2i | 2.0839 | Ir2—C2i | 2.3616 |
Ir2—C1 | 2.2984 | | |
| | | |
C2—Ir1—C5 | 161.15 | C1—Ir2—C2i | 63.54 |
C2—Ir1—C2i | 78.55 | C1i—Ir2—C2 | 63.54 |
C2—Ir1—C5i | 97.31 | C2—Ir2—C2i | 67.92 |
C2—Ir1—C5ii | 161.15 | C1i—Ir2—C2i | 35.9 |
C2—Ir1—C5iii | 97.31 | Ir2—C1—C2 | 74.45 |
C2i—Ir1—C5 | 97.31 | Ir2—C1—Ir2i | 114.37 |
C5—Ir1—C5i | 92.19 | Ir2—C1—C1i | 70.96 |
C5—Ir1—C5ii | 36.98 | Ir2i—C1—C2 | 74.45 |
C5—Ir1—C5iii | 80.62 | Ir2i—C1—C1i | 70.96 |
C2i—Ir1—C5i | 161.15 | Ir1—C2—Ir2 | 75.7 |
C2i—Ir1—C5ii | 97.31 | Ir1—C2—C1 | 117.39 |
C2i—Ir1—C5iii | 161.15 | Ir1—C2—Ir2i | 75.7 |
C5i—Ir1—C5ii | 80.62 | Ir2—C2—C1 | 69.65 |
C5i—Ir1—C5iii | 36.98 | Ir2—C2—Ir2i | 109.76 |
C5ii—Ir1—C5iii | 92.19 | Ir2i—C2—C1 | 69.65 |
C1—Ir2—C2 | 35.9 | Ir1—C5—C6 | 113.59 |
C1—Ir2—C1i | 38.08 | Ir1—C5—C5ii | 71.51 |
Symmetry codes: (i) −x, y, −z+1/2; (ii) x, y, −z+1/2; (iii) −x, y, z. |
Selected geometric parameters (Å, º) for (28) topCl1—C48 | 1.6462 | Cl5—C47 | 1.8563 |
Cl1—C47 | 1.5467 | Cl5—C48 | 1.868 |
Cl1—Cl2 | 0.6374 | Cl7—C48 | 1.8438 |
Cl2—C47 | 1.687 | Cl7—Cl8 | 0.4449 |
Cl2—C48 | 1.8113 | Cl7—C47 | 1.8483 |
Cl4—Cl5 | 0.3526 | Cl8—C47 | 1.6216 |
Cl4—C47 | 1.6988 | Cl8—C48 | 1.5856 |
Cl4—C48 | 1.7361 | | |
| | | |
C47—Cl1—C48 | 3.96 | Cl4—C47—Cl7 | 109.82 |
Cl2—Cl1—C48 | 94.5 | Cl4—C47—Cl8 | 109.93 |
Cl2—Cl1—C47 | 91.38 | Cl4—C47—C48 | 102.14 |
Cl1—Cl2—C48 | 64.96 | Cl5—C47—Cl7 | 106.99 |
Cl1—Cl2—C47 | 66.43 | Cl5—C47—Cl8 | 104.93 |
C47—Cl2—C48 | 2.66 | Cl5—C47—C48 | 92.26 |
Cl5—Cl4—C48 | 106.68 | Cl7—C47—Cl8 | 12.7 |
Cl5—Cl4—C47 | 111.33 | Cl7—C47—C48 | 85.95 |
C47—Cl4—C48 | 4.79 | Cl8—C47—C48 | 73.4 |
Cl4—Cl5—C48 | 62.9 | Cl1—C48—Cl2 | 20.54 |
C47—Cl5—C48 | 4.55 | Cl1—C48—Cl4 | 115.05 |
Cl4—Cl5—C47 | 58.48 | Cl1—C48—Cl5 | 125.42 |
C47—Cl7—C48 | 4.6 | Cl1—C48—Cl7 | 93.3 |
Cl8—Cl7—C47 | 53.23 | Cl1—C48—Cl8 | 103.01 |
Cl8—Cl7—C48 | 48.68 | Cl1—C48—C47 | 45.98 |
C47—Cl8—C48 | 5.15 | Cl2—C48—Cl4 | 94.91 |
Cl7—Cl8—C48 | 119.15 | Cl2—C48—Cl5 | 105.18 |
Cl7—Cl8—C47 | 114.07 | Cl2—C48—Cl7 | 104.45 |
Cl1—C47—Cl2 | 22.19 | Cl2—C48—Cl8 | 115.9 |
Cl1—C47—Cl4 | 123.04 | Cl2—C48—C47 | 31.82 |
Cl1—C47—Cl5 | 133.13 | Cl4—C48—Cl5 | 10.42 |
Cl1—C47—Cl7 | 96.53 | Cl4—C48—Cl7 | 108.37 |
Cl1—C47—Cl8 | 105.94 | Cl4—C48—Cl8 | 109.81 |
Cl1—C47—C48 | 130.06 | Cl4—C48—C47 | 73.07 |
Cl2—C47—Cl4 | 101.07 | Cl5—C48—Cl7 | 106.69 |
Cl2—C47—Cl5 | 111.06 | Cl5—C48—Cl8 | 105.9 |
Cl2—C47—Cl7 | 109.54 | Cl5—C48—C47 | 83.19 |
Cl2—C47—Cl8 | 121.12 | Cl7—C48—Cl8 | 12.16 |
Cl2—C47—C48 | 145.52 | Cl7—C48—C47 | 89.44 |
Cl4—C47—Cl5 | 10.19 | Cl8—C48—C47 | 101.45 |
Selected geometric parameters (Å, º) for (29) topTc1—N1 | 2.0066 | N1—C1 | 1.354 |
Tc1—N2 | 2.0108 | N2—C6 | 1.3353 |
Tc1—N5 | 2.0056 | N5—C13 | 1.3418 |
| | | |
N1—Tc1—N2 | 76.34 | N1i—Tc1—N2i | 76.34 |
N1—Tc1—N5 | 86.5 | N1i—Tc1—N5i | 86.5 |
N1—Tc1—N1i | 137.57 | N2i—Tc1—N5i | 137.95 |
N1—Tc1—N2i | 85.91 | Tc1—N1—C1 | 118.26 |
N1—Tc1—N5i | 129.22 | Tc1—N2—C6 | 117.68 |
N2—Tc1—N5 | 137.95 | Tc1—N5—C13 | 120.21 |
N1i—Tc1—N2 | 85.91 | N1—C1—C2 | 127.3 |
N2—Tc1—N2i | 129.71 | N1—C1—C6 | 112.35 |
N2—Tc1—N5i | 85.89 | N2—C6—C1 | 114.71 |
N1i—Tc1—N5 | 129.22 | N2—C6—C5 | 125.25 |
N2i—Tc1—N5 | 85.89 | N5—C13—C14 | 129.21 |
N5—Tc1—N5i | 75.75 | N5—C13—C13i | 111.92 |
Symmetry code: (i) x, −y+3/2, −z+1/2. |
Selected geometric parameters (Å, º) for (30) topPd1—Cl1 | 2.2949 (6) | Pd1—Cl1ii | 2.2949 (6) |
Pd1—N1 | 2.0590 (5) | N1—C1 | 1.4740 (4) |
Pd1—N1i | 2.0590 (5) | | |
| | | |
Cl1—Pd1—N1 | 90.00 (3) | Cl1ii—Pd1—N1 | 90.00 (3) |
Cl1—Pd1—N1i | 90.00 (3) | Cl1ii—Pd1—N1i | 90.00 (3) |
Cl1—Pd1—Cl1ii | 180 | Pd1—N1—C1 | 111.22 (3) |
N1—Pd1—N1i | 180 | N1—C1—C2 | 113.27 (3) |
Symmetry codes: (i) −x, y, −z+2; (ii) −x, −y, −z+2. |
Hydrogen-bond geometry (Å, º) for (30) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···Cl1iii | 0.9 | 2.61 | 3.4362 (9) | 153 |
N1—H1···Cl1iv | 0.9 | 2.61 | 3.4362 (9) | 153 |
Symmetry codes: (iii) −x+1/2, −y+1/2, −z+2; (iv) x+1/2, −y+1/2, z. |