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Eight new structures of dirhodium complexes, each with four biimidazole (H2bim) ligands, were obtained: [Rh2(H2bim)4(H2O)2](NO3)4·4H2O (I), [Rh2(H2bim)4(H2O)2](ClO4)4·5H2O (II), [Rh2(H2bim)4(MeOH)2](ClO4)4 (III), [Rh2(H2bim)4(DMF)2](BF4)4 (IV), [Rh2(H2bim)4(Mepy)2](SiF6)2·8H2O (V), [{Rh2(H2bim)4(pz)}2(μ-pz)](SiF6)(ClO4)6·12.7H2O (VI), [{Rh2(H2bim)4(pz)}2(μ-pz)](ClO4)8·11.4H2O (VII) and [Rh2(H2bim)4(μ-pz)](SiF6)2·6H2O (VIII). The unbridged Rh—Rh bond distances range between 2.6313 (8) and 2.7052 (5) Å. The dirhodium units adopt a staggered conformation with torsion angles N—Rh—Rh—N of 37.6 (4)–48.98 (8)°. Various assembled structures were constructed by hydrogen bonding between the complexes and the anions: a discrete structure in (IV), one-dimensional structure in (II), two-dimensional structures in (I), (III), (VI), (VII) and (VIII) and a three-dimensional structure in (V).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520614021428/ry5061sup1.cif
Contains datablocks I, II, III, IV, V, VI, VII, VIII

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614021428/ry5061Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614021428/ry5061IIsup3.hkl
Contains datablock jin113

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614021428/ry5061IIIsup4.hkl
Contains datablock jin103

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614021428/ry5061IVsup5.hkl
Contains datablock jin100_2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614021428/ry5061Vsup6.hkl
Contains datablock V

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614021428/ry5061VIsup7.hkl
Contains datablock jin117

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614021428/ry5061VIIsup8.hkl
Contains datablock vii

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520614021428/ry5061VIIIsup9.hkl
Contains datablock jin160

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520614021428/ry5061sup10.pdf
IR spectra, close contacts

CCDC references: 1026431; 1026432; 1026433; 1026434; 1026435; 1026436; 1026437; 1026438

Experimental top

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1.

Results and discussion top

Computing details top

For all compounds, data collection: CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2008); software used to prepare material for publication: Yadokari-XG 2009 (Wakita, Nemoto et al., 2009).

(I) top
Crystal data top
C24H28N16O2Rh2·4(NO3)·4(H2O)Dx = 1.891 Mg m3
Mr = 1098.55Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, PbcnCell parameters from 9401 reflections
a = 18.843 (3) Åθ = 3.0–27.5°
b = 16.642 (3) ŵ = 0.96 mm1
c = 12.307 (2) ÅT = 123 K
V = 3859.2 (11) Å3Prismatic, green
Z = 40.66 × 0.12 × 0.10 mm
F(000) = 2216
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
4413 independent reflections
Radiation source: rotating-anode X-ray tube4134 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.2°
ω scansh = 2417
Absorption correction: numerical
NUMABS (Higashi, 1999)
k = 2119
Tmin = 0.809, Tmax = 0.956l = 1511
29049 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.080H atoms treated by a mixture of independent and constrained refinement
S = 1.32 w = 1/[σ2(Fo2) + (0.0208P)2 + 3.7755P]
where P = (Fo2 + 2Fc2)/3
4416 reflections(Δ/σ)max = 0.001
313 parametersΔρmax = 0.79 e Å3
0 restraintsΔρmin = 0.57 e Å3
Crystal data top
C24H28N16O2Rh2·4(NO3)·4(H2O)V = 3859.2 (11) Å3
Mr = 1098.55Z = 4
Orthorhombic, PbcnMo Kα radiation
a = 18.843 (3) ŵ = 0.96 mm1
b = 16.642 (3) ÅT = 123 K
c = 12.307 (2) Å0.66 × 0.12 × 0.10 mm
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
4413 independent reflections
Absorption correction: numerical
NUMABS (Higashi, 1999)
4134 reflections with I > 2σ(I)
Tmin = 0.809, Tmax = 0.956Rint = 0.042
29049 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0440 restraints
wR(F2) = 0.080H atoms treated by a mixture of independent and constrained refinement
S = 1.32Δρmax = 0.79 e Å3
4416 reflectionsΔρmin = 0.57 e Å3
313 parameters
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 not 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
xyzUiso*/Ueq
Rh10.496293 (11)0.284327 (13)0.641384 (16)0.01116 (7)
N10.59822 (13)0.32611 (15)0.62505 (18)0.0135 (5)
C10.64592 (15)0.26794 (19)0.6126 (2)0.0150 (6)
N20.71109 (13)0.29788 (15)0.59918 (19)0.0171 (5)
H2N0.75040.27010.59080.021*
C20.70526 (16)0.38076 (19)0.6009 (2)0.0195 (6)
H20.74260.41860.59270.023*
C30.63508 (16)0.39728 (18)0.6166 (2)0.0161 (6)
H30.61490.44950.62110.019*
N30.55025 (13)0.17784 (15)0.63014 (18)0.0140 (5)
C40.61985 (16)0.18639 (19)0.6143 (2)0.0151 (6)
N40.65146 (14)0.11611 (16)0.59794 (19)0.0189 (6)
H4N0.69690.10830.58520.023*
C50.60030 (17)0.0581 (2)0.6046 (2)0.0216 (7)
H50.60700.00180.59680.026*
C60.53747 (17)0.09677 (19)0.6246 (2)0.0186 (6)
H60.49260.07170.63330.022*
N50.44123 (13)0.39047 (15)0.64183 (17)0.0134 (5)
C70.37062 (15)0.38177 (19)0.6380 (2)0.0151 (6)
N60.33816 (14)0.45272 (16)0.63229 (18)0.0183 (5)
H6N0.29210.46080.62910.022*
C80.38953 (17)0.5106 (2)0.6324 (2)0.0197 (6)
H80.38230.56700.62940.024*
C90.45320 (17)0.47192 (19)0.6375 (2)0.0176 (6)
H90.49840.49710.63800.021*
N70.39421 (13)0.24234 (15)0.64234 (18)0.0138 (5)
C100.34518 (16)0.30002 (19)0.6403 (2)0.0156 (6)
N80.27952 (13)0.26823 (17)0.63876 (19)0.0194 (6)
H8N0.23920.29500.63770.023*
C110.28727 (17)0.1858 (2)0.6392 (2)0.0205 (7)
H110.25010.14710.63880.025*
C120.35840 (16)0.17020 (19)0.6402 (2)0.0170 (6)
H120.37960.11840.63940.020*
O10.49336 (12)0.28149 (15)0.45463 (17)0.0175 (4)
H1A0.465 (2)0.316 (3)0.433 (3)0.045 (13)*
H1B0.4778 (19)0.241 (2)0.436 (3)0.020 (10)*
N90.84385 (14)0.12376 (17)0.61933 (19)0.0211 (6)
O20.83313 (13)0.19829 (15)0.61922 (19)0.0303 (6)
O30.79334 (13)0.07548 (17)0.6175 (2)0.0383 (6)
O40.90598 (11)0.09783 (14)0.62123 (17)0.0235 (5)
N100.14816 (15)0.44192 (18)0.6615 (2)0.0246 (6)
O50.19275 (12)0.48324 (16)0.61076 (19)0.0310 (6)
O60.16805 (15)0.38192 (16)0.7156 (2)0.0397 (7)
O70.08408 (13)0.46105 (16)0.65985 (19)0.0312 (6)
O80.12766 (14)0.21130 (17)0.6437 (2)0.0309 (6)
H8A0.088 (3)0.216 (3)0.618 (4)0.072 (18)*
H8B0.117 (3)0.227 (3)0.709 (4)0.070 (17)*
O90.45282 (18)0.13651 (18)0.3771 (2)0.0390 (7)
H9A0.495 (3)0.116 (4)0.358 (4)0.10 (3)*
H9B0.423 (3)0.130 (3)0.327 (4)0.073 (18)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.00905 (12)0.01098 (12)0.01346 (11)0.00023 (8)0.00001 (8)0.00033 (8)
N10.0118 (12)0.0141 (13)0.0145 (11)0.0007 (10)0.0005 (9)0.0008 (9)
C10.0121 (14)0.0179 (16)0.0149 (13)0.0021 (12)0.0004 (10)0.0017 (11)
N20.0122 (13)0.0193 (15)0.0197 (12)0.0003 (11)0.0018 (9)0.0020 (10)
C20.0152 (15)0.0201 (17)0.0231 (15)0.0038 (13)0.0015 (12)0.0006 (12)
C30.0186 (15)0.0128 (16)0.0167 (14)0.0022 (12)0.0007 (11)0.0016 (11)
N30.0129 (12)0.0121 (13)0.0171 (11)0.0009 (10)0.0003 (9)0.0012 (9)
C40.0135 (15)0.0170 (16)0.0148 (13)0.0028 (12)0.0008 (11)0.0021 (11)
N40.0133 (13)0.0190 (15)0.0245 (13)0.0042 (11)0.0033 (10)0.0016 (10)
C50.0226 (17)0.0136 (16)0.0286 (16)0.0007 (13)0.0040 (12)0.0003 (12)
C60.0179 (16)0.0150 (16)0.0229 (15)0.0003 (12)0.0019 (12)0.0014 (12)
N50.0128 (12)0.0138 (13)0.0136 (11)0.0012 (10)0.0006 (9)0.0006 (9)
C70.0124 (14)0.0219 (17)0.0109 (12)0.0012 (12)0.0014 (10)0.0001 (11)
N60.0164 (13)0.0192 (14)0.0191 (12)0.0054 (11)0.0005 (10)0.0016 (10)
C80.0232 (17)0.0161 (17)0.0198 (14)0.0023 (13)0.0004 (12)0.0006 (12)
C90.0199 (16)0.0154 (16)0.0175 (13)0.0016 (12)0.0013 (11)0.0004 (12)
N70.0115 (12)0.0147 (13)0.0154 (11)0.0013 (10)0.0010 (9)0.0010 (9)
C100.0124 (14)0.0219 (17)0.0124 (13)0.0015 (12)0.0010 (10)0.0004 (11)
N80.0106 (12)0.0265 (16)0.0211 (13)0.0000 (11)0.0023 (10)0.0012 (11)
C110.0177 (16)0.0230 (18)0.0209 (15)0.0061 (13)0.0037 (12)0.0008 (12)
C120.0185 (16)0.0135 (16)0.0189 (14)0.0038 (12)0.0006 (11)0.0009 (12)
O10.0188 (12)0.0146 (12)0.0191 (10)0.0006 (11)0.0034 (8)0.0023 (9)
N90.0189 (14)0.0251 (16)0.0192 (13)0.0056 (12)0.0019 (10)0.0018 (11)
O20.0278 (14)0.0243 (14)0.0387 (14)0.0104 (11)0.0004 (10)0.0032 (10)
O30.0166 (13)0.0301 (16)0.0682 (18)0.0006 (11)0.0009 (12)0.0007 (13)
O40.0130 (11)0.0236 (13)0.0339 (12)0.0050 (9)0.0020 (9)0.0058 (10)
N100.0187 (15)0.0254 (16)0.0297 (14)0.0028 (12)0.0048 (11)0.0067 (12)
O50.0195 (13)0.0347 (16)0.0390 (14)0.0026 (11)0.0030 (10)0.0006 (11)
O60.0371 (16)0.0309 (16)0.0512 (15)0.0140 (13)0.0038 (12)0.0083 (12)
O70.0176 (12)0.0341 (15)0.0419 (14)0.0075 (11)0.0006 (10)0.0036 (11)
O80.0206 (14)0.0416 (17)0.0306 (14)0.0014 (12)0.0053 (11)0.0027 (12)
O90.0394 (18)0.0331 (17)0.0445 (16)0.0040 (14)0.0044 (14)0.0108 (13)
Geometric parameters (Å, º) top
Rh1—N72.047 (2)C7—C101.443 (4)
Rh1—N32.048 (2)N6—C81.365 (4)
Rh1—N52.049 (2)N6—H6N0.8800
Rh1—N12.053 (2)C8—C91.363 (4)
Rh1—O12.299 (2)C8—H80.9500
Rh1—Rh1i2.6771 (6)C9—H90.9500
N1—C11.330 (4)N7—C101.333 (4)
N1—C31.377 (4)N7—C121.377 (4)
C1—N21.336 (4)C10—N81.346 (4)
C1—C41.443 (4)N8—C111.380 (4)
N2—C21.384 (4)N8—H8N0.8800
N2—H2N0.8800C11—C121.365 (4)
C2—C31.365 (4)C11—H110.9500
C2—H20.9500C12—H120.9500
C3—H30.9500O1—H1A0.83 (5)
N3—C41.333 (4)O1—H1B0.78 (4)
N3—C61.372 (4)N9—O31.246 (4)
C4—N41.328 (4)N9—O41.248 (3)
N4—C51.367 (4)N9—O21.257 (4)
N4—H4N0.8800N10—O71.249 (3)
C5—C61.370 (4)N10—O51.253 (4)
C5—H50.9500N10—O61.257 (4)
C6—H60.9500O8—H8A0.81 (6)
N5—C71.339 (4)O8—H8B0.87 (5)
N5—C91.375 (4)O9—H9A0.90 (6)
C7—N61.332 (4)O9—H9B0.83 (5)
N7—Rh1—N399.88 (10)C5—C6—H6125.7
N7—Rh1—N579.53 (10)N3—C6—H6125.7
N3—Rh1—N5176.24 (9)C7—N5—C9105.6 (3)
N7—Rh1—N1174.71 (9)C7—N5—Rh1114.2 (2)
N3—Rh1—N179.74 (10)C9—N5—Rh1140.1 (2)
N5—Rh1—N1100.49 (10)N6—C7—N5111.2 (3)
N7—Rh1—O188.63 (8)N6—C7—C10133.2 (3)
N3—Rh1—O185.80 (9)N5—C7—C10115.6 (3)
N5—Rh1—O190.47 (9)C7—N6—C8107.4 (3)
N1—Rh1—O186.07 (8)C7—N6—H6N126.3
N7—Rh1—Rh1i92.48 (6)C8—N6—H6N126.3
N3—Rh1—Rh1i92.38 (6)C9—C8—N6107.0 (3)
N5—Rh1—Rh1i91.36 (6)C9—C8—H8126.5
N1—Rh1—Rh1i92.81 (6)N6—C8—H8126.5
O1—Rh1—Rh1i178.00 (6)C8—C9—N5108.8 (3)
C1—N1—C3106.1 (2)C8—C9—H9125.6
C1—N1—Rh1113.4 (2)N5—C9—H9125.6
C3—N1—Rh1140.4 (2)C10—N7—C12106.7 (2)
N1—C1—N2111.4 (3)C10—N7—Rh1113.9 (2)
N1—C1—C4116.9 (3)C12—N7—Rh1139.3 (2)
N2—C1—C4131.7 (3)N7—C10—N8110.8 (3)
C1—N2—C2107.3 (3)N7—C10—C7116.7 (3)
C1—N2—H2N126.4N8—C10—C7132.5 (3)
C2—N2—H2N126.4C10—N8—C11107.1 (3)
C3—C2—N2106.2 (3)C10—N8—H8N126.5
C3—C2—H2126.9C11—N8—H8N126.5
N2—C2—H2126.9C12—C11—N8107.0 (3)
C2—C3—N1109.0 (3)C12—C11—H11126.5
C2—C3—H3125.5N8—C11—H11126.5
N1—C3—H3125.5C11—C12—N7108.4 (3)
C4—N3—C6105.7 (3)C11—C12—H12125.8
C4—N3—Rh1113.9 (2)N7—C12—H12125.8
C6—N3—Rh1140.1 (2)Rh1—O1—H1A109 (3)
N4—C4—N3111.7 (3)Rh1—O1—H1B109 (3)
N4—C4—C1132.3 (3)H1A—O1—H1B105 (4)
N3—C4—C1115.9 (3)O3—N9—O4119.6 (3)
C4—N4—C5107.3 (3)O3—N9—O2120.9 (3)
C4—N4—H4N126.4O4—N9—O2119.5 (3)
C5—N4—H4N126.4O7—N10—O5120.0 (3)
N4—C5—C6106.8 (3)O7—N10—O6120.0 (3)
N4—C5—H5126.6O5—N10—O6120.0 (3)
C6—C5—H5126.6H8A—O8—H8B97 (4)
C5—C6—N3108.6 (3)H9A—O9—H9B110 (5)
N1—Rh1—Rh1i—N5i39.77 (10)Rh1—N3—C6—C5172.7 (2)
N3—Rh1—Rh1i—N7i40.03 (10)N7—Rh1—N5—C72.58 (18)
N7—Rh1—N1—C184.5 (11)N3—Rh1—N5—C778.8 (15)
N3—Rh1—N1—C11.87 (18)N1—Rh1—N5—C7172.04 (18)
N5—Rh1—N1—C1174.31 (18)O1—Rh1—N5—C785.94 (19)
O1—Rh1—N1—C184.56 (19)Rh1i—Rh1—N5—C794.85 (18)
Rh1i—Rh1—N1—C193.79 (18)N7—Rh1—N5—C9176.7 (3)
N7—Rh1—N1—C390.7 (11)N3—Rh1—N5—C995.3 (15)
N3—Rh1—N1—C3177.1 (3)N1—Rh1—N5—C92.0 (3)
N5—Rh1—N1—C30.9 (3)O1—Rh1—N5—C988.1 (3)
O1—Rh1—N1—C390.7 (3)Rh1i—Rh1—N5—C991.1 (3)
Rh1i—Rh1—N1—C391.0 (3)C9—N5—C7—N60.4 (3)
C3—N1—C1—N21.4 (3)Rh1—N5—C7—N6176.45 (17)
Rh1—N1—C1—N2178.23 (18)C9—N5—C7—C10179.3 (2)
C3—N1—C1—C4177.9 (2)Rh1—N5—C7—C103.3 (3)
Rh1—N1—C1—C41.1 (3)N5—C7—N6—C80.0 (3)
N1—C1—N2—C21.3 (3)C10—C7—N6—C8179.7 (3)
C4—C1—N2—C2177.9 (3)C7—N6—C8—C90.4 (3)
C1—N2—C2—C30.6 (3)N6—C8—C9—N50.7 (3)
N2—C2—C3—N10.3 (3)C7—N5—C9—C80.7 (3)
C1—N1—C3—C21.0 (3)Rh1—N5—C9—C8175.0 (2)
Rh1—N1—C3—C2176.4 (2)N3—Rh1—N7—C10174.82 (19)
N7—Rh1—N3—C4172.17 (19)N5—Rh1—N7—C101.40 (18)
N5—Rh1—N3—C491.4 (15)N1—Rh1—N7—C1089.4 (11)
N1—Rh1—N3—C42.47 (19)O1—Rh1—N7—C1089.33 (19)
O1—Rh1—N3—C484.29 (19)Rh1i—Rh1—N7—C1092.33 (18)
Rh1i—Rh1—N3—C494.90 (19)N3—Rh1—N7—C121.8 (3)
N7—Rh1—N3—C60.6 (3)N5—Rh1—N7—C12178.0 (3)
N5—Rh1—N3—C681.3 (15)N1—Rh1—N7—C1287.2 (11)
N1—Rh1—N3—C6175.2 (3)O1—Rh1—N7—C1287.3 (3)
O1—Rh1—N3—C688.4 (3)Rh1i—Rh1—N7—C1291.1 (3)
Rh1i—Rh1—N3—C692.4 (3)C12—N7—C10—N81.0 (3)
C6—N3—C4—N40.7 (3)Rh1—N7—C10—N8178.68 (17)
Rh1—N3—C4—N4174.43 (18)C12—N7—C10—C7177.8 (2)
C6—N3—C4—C1177.8 (2)Rh1—N7—C10—C70.1 (3)
Rh1—N3—C4—C12.7 (3)N6—C7—C10—N7177.5 (3)
N1—C1—C4—N4175.3 (3)N5—C7—C10—N72.2 (4)
N2—C1—C4—N43.8 (5)N6—C7—C10—N80.9 (5)
N1—C1—C4—N31.1 (4)N5—C7—C10—N8179.4 (3)
N2—C1—C4—N3179.8 (3)N7—C10—N8—C110.3 (3)
N3—C4—N4—C50.7 (3)C7—C10—N8—C11178.2 (3)
C1—C4—N4—C5177.2 (3)C10—N8—C11—C120.5 (3)
C4—N4—C5—C60.4 (3)N8—C11—C12—N71.1 (3)
N4—C5—C6—N30.0 (3)C10—N7—C12—C111.3 (3)
C4—N3—C6—C50.5 (3)Rh1—N7—C12—C11178.0 (2)
Symmetry code: (i) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O20.881.992.845 (3)162
N4—H4N···O30.881.942.768 (4)157
N6—H6N···O50.881.922.799 (4)175
N8—H8N···O60.882.192.981 (4)149
N8—H8N···O80.882.523.015 (4)116
O1—H1A···N9ii0.83 (5)2.57 (5)3.354 (4)158 (4)
O1—H1A···O2ii0.83 (5)2.57 (4)3.171 (3)130 (4)
O1—H1A···O4ii0.83 (5)1.93 (5)2.760 (3)174 (4)
O1—H1B···O90.78 (4)1.93 (4)2.705 (4)171 (4)
O8—H8A···O1ii0.81 (6)2.00 (6)2.808 (3)174 (5)
O8—H8B···O2i0.87 (5)2.36 (5)3.017 (4)133 (4)
O9—H9A···O7iii0.90 (6)2.12 (7)2.993 (4)164 (6)
O9—H9B···O6iv0.83 (5)2.21 (6)3.038 (4)170 (5)
O9—H9B···O7iv0.83 (5)2.56 (5)3.204 (4)135 (5)
Symmetry codes: (i) x+1, y, z+3/2; (ii) x1/2, y+1/2, z+1; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y+1/2, z1/2.
(II) top
Crystal data top
C24H28N16O2Rh2·4(ClO4)·5(H2O)F(000) = 2544
Mr = 1266.32Dx = 1.884 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
a = 13.453 (2) ÅCell parameters from 11005 reflections
b = 13.334 (2) Åθ = 3.0–27.5°
c = 24.906 (4) ŵ = 1.08 mm1
β = 91.749 (2)°T = 296 K
V = 4465.5 (13) Å3Prismatic, green
Z = 40.41 × 0.35 × 0.34 mm
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
10190 independent reflections
Radiation source: rotating-anode X-ray tube8188 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.0°
ω scansh = 1716
Absorption correction: numerical
NUMABS (Higashi, 1999)
k = 1417
Tmin = 0.731, Tmax = 0.815l = 3231
34616 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.058Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.163H atoms treated by a mixture of independent and constrained refinement
S = 1.08 w = 1/[σ2(Fo2) + (0.0753P)2 + 6.5586P]
where P = (Fo2 + 2Fc2)/3
10190 reflections(Δ/σ)max = 0.001
641 parametersΔρmax = 0.78 e Å3
0 restraintsΔρmin = 0.74 e Å3
Crystal data top
C24H28N16O2Rh2·4(ClO4)·5(H2O)V = 4465.5 (13) Å3
Mr = 1266.32Z = 4
Monoclinic, P21/nMo Kα radiation
a = 13.453 (2) ŵ = 1.08 mm1
b = 13.334 (2) ÅT = 296 K
c = 24.906 (4) Å0.41 × 0.35 × 0.34 mm
β = 91.749 (2)°
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
10190 independent reflections
Absorption correction: numerical
NUMABS (Higashi, 1999)
8188 reflections with I > 2σ(I)
Tmin = 0.731, Tmax = 0.815Rint = 0.034
34616 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0580 restraints
wR(F2) = 0.163H atoms treated by a mixture of independent and constrained refinement
S = 1.08Δρmax = 0.78 e Å3
10190 reflectionsΔρmin = 0.74 e Å3
641 parameters
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 not 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
xyzUiso*/UeqOcc. (<1)
Rh10.53955 (2)0.26880 (3)0.600046 (13)0.03340 (11)
Rh20.69975 (2)0.26866 (3)0.664573 (14)0.03684 (12)
N10.4434 (3)0.2821 (3)0.66190 (15)0.0390 (8)
C10.4049 (3)0.1948 (4)0.6768 (2)0.0447 (10)
N20.3366 (3)0.2092 (4)0.7139 (2)0.0639 (13)
H2N0.30230.16310.72870.077*
C20.3304 (4)0.3090 (5)0.7241 (3)0.0698 (17)
H20.28920.34010.74840.084*
C30.3976 (4)0.3550 (4)0.6912 (2)0.0536 (12)
H30.40970.42350.68930.064*
N30.5097 (3)0.1203 (3)0.61424 (15)0.0396 (8)
C40.4409 (3)0.1066 (4)0.6505 (2)0.0442 (10)
N40.4204 (3)0.0088 (3)0.65627 (19)0.0543 (11)
H4N0.37830.01670.67770.065*
C50.4781 (4)0.0421 (4)0.6223 (2)0.0582 (13)
H50.47990.11130.61780.070*
C60.5336 (4)0.0268 (4)0.5956 (2)0.0506 (12)
H60.57940.01280.56950.061*
N50.5593 (2)0.4171 (3)0.58141 (14)0.0364 (8)
C70.6056 (3)0.4311 (3)0.53579 (18)0.0385 (9)
N60.6104 (3)0.5293 (3)0.52416 (16)0.0436 (9)
H6N0.63750.55560.49670.052*
C80.5643 (3)0.5798 (4)0.5641 (2)0.0463 (11)
H80.55570.64880.56680.056*
C90.5337 (3)0.5098 (4)0.59883 (19)0.0428 (10)
H90.50010.52300.63010.051*
N70.6206 (3)0.2559 (3)0.53224 (15)0.0390 (8)
C100.6384 (3)0.3432 (4)0.50845 (17)0.0396 (9)
N80.6826 (3)0.3280 (3)0.46160 (17)0.0536 (10)
H8N0.70160.37360.43980.064*
C110.6920 (4)0.2273 (4)0.4549 (2)0.0585 (14)
H110.71950.19530.42570.070*
C120.6539 (4)0.1817 (4)0.4986 (2)0.0504 (11)
H120.65090.11300.50470.061*
N90.6384 (3)0.3734 (3)0.71439 (15)0.0423 (8)
C130.5952 (4)0.3336 (4)0.7567 (2)0.0512 (12)
N100.5627 (4)0.4057 (4)0.78885 (18)0.0664 (13)
H10N0.53190.39700.81820.080*
C140.5871 (5)0.4961 (5)0.7667 (2)0.0676 (16)
H140.57380.55950.78040.081*
C150.6344 (4)0.4748 (4)0.7210 (2)0.0531 (12)
H150.66010.52200.69760.064*
N110.6335 (3)0.1765 (3)0.71885 (15)0.0453 (9)
C160.5913 (4)0.2257 (4)0.7586 (2)0.0502 (12)
N120.5527 (3)0.1611 (4)0.79328 (18)0.0635 (12)
H12N0.52120.17650.82170.076*
C170.5720 (4)0.0677 (5)0.7758 (2)0.0627 (15)
H170.55390.00820.79240.075*
C180.6224 (4)0.0763 (4)0.7299 (2)0.0520 (12)
H180.64560.02340.70930.062*
N130.7779 (3)0.3618 (3)0.61590 (15)0.0396 (8)
C190.8386 (3)0.3131 (4)0.58366 (19)0.0442 (10)
N140.8953 (3)0.3771 (4)0.55698 (18)0.0559 (11)
H14N0.93920.36180.53400.067*
C200.8703 (4)0.4718 (4)0.5732 (2)0.0602 (14)
H200.89760.53170.56140.072*
C210.7992 (4)0.4617 (4)0.6093 (2)0.0489 (11)
H210.76890.51430.62710.059*
N150.7704 (3)0.1651 (3)0.61760 (16)0.0429 (8)
C220.8347 (3)0.2059 (4)0.5846 (2)0.0448 (10)
N160.8832 (3)0.1360 (4)0.55801 (19)0.0566 (11)
H16N0.92730.14600.53430.068*
C230.8496 (4)0.0443 (4)0.5755 (2)0.0610 (14)
H230.87040.01850.56410.073*
C240.7804 (4)0.0632 (4)0.6123 (2)0.0519 (12)
H240.74540.01510.63110.062*
O10.3963 (3)0.2753 (3)0.54537 (15)0.0538 (9)
O20.8362 (3)0.2659 (4)0.72130 (19)0.0794 (14)
Cl10.82216 (13)0.56104 (17)0.41178 (8)0.0877 (6)
O30.7225 (3)0.5342 (4)0.4201 (2)0.0953 (16)
O40.8275 (8)0.6651 (8)0.4169 (5)0.251 (6)
O50.8534 (5)0.5347 (7)0.3606 (3)0.147 (3)
O60.8836 (5)0.5176 (10)0.4482 (3)0.226 (6)
Cl20.62259 (12)0.29621 (12)0.31100 (6)0.0670 (4)
O70.6129 (5)0.3492 (7)0.2641 (3)0.176 (4)
O80.7027 (8)0.3402 (10)0.3378 (3)0.247 (7)
O90.5418 (6)0.2932 (5)0.3436 (4)0.160 (3)
O100.6425 (7)0.1999 (5)0.3012 (5)0.220 (5)
Cl30.37165 (15)0.4949 (2)0.89392 (11)0.1040 (7)
O110.4298 (10)0.4154 (12)0.8840 (6)0.288 (7)
O120.2801 (5)0.4730 (9)0.8978 (6)0.280 (8)
O130.3977 (9)0.5226 (14)0.9437 (4)0.312 (9)
O140.4004 (10)0.5565 (10)0.8582 (5)0.260 (6)
Cl4A0.7636 (3)0.2821 (2)0.87174 (16)0.0626 (10)0.649 (8)
O15A0.7851 (6)0.3493 (5)0.8278 (3)0.081 (2)0.649 (8)
Cl4B0.7282 (6)0.2572 (5)0.8980 (4)0.081 (2)0.351 (8)
O15B0.7235 (13)0.1923 (12)0.9389 (8)0.119 (7)0.351 (8)
O160.6564 (5)0.3039 (5)0.8873 (3)0.123 (2)
O170.7675 (5)0.1868 (4)0.8526 (3)0.113 (2)
O180.8267 (5)0.3083 (5)0.9135 (2)0.121 (2)
O190.2799 (5)0.0158 (4)0.7481 (2)0.115 (2)
O200.4216 (6)0.2069 (7)0.8760 (3)0.168 (3)
O211.0149 (5)0.2533 (5)0.4893 (3)0.116 (2)
O220.3310 (4)0.0906 (4)0.5107 (2)0.1086 (18)
O231.0140 (5)0.2828 (8)0.6767 (4)0.215 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.03611 (18)0.0295 (2)0.03494 (19)0.00147 (12)0.00621 (13)0.00278 (12)
Rh20.03811 (19)0.0351 (2)0.0374 (2)0.00114 (13)0.00349 (14)0.00125 (13)
N10.0418 (18)0.035 (2)0.041 (2)0.0015 (15)0.0098 (15)0.0033 (15)
C10.042 (2)0.042 (3)0.051 (3)0.000 (2)0.0099 (19)0.011 (2)
N20.062 (3)0.054 (3)0.078 (3)0.001 (2)0.038 (2)0.014 (2)
C20.076 (4)0.056 (4)0.080 (4)0.016 (3)0.045 (3)0.010 (3)
C30.057 (3)0.046 (3)0.059 (3)0.005 (2)0.018 (2)0.001 (2)
N30.0424 (18)0.033 (2)0.043 (2)0.0018 (15)0.0060 (15)0.0052 (16)
C40.042 (2)0.040 (3)0.051 (3)0.0022 (19)0.0051 (19)0.009 (2)
N40.054 (2)0.035 (2)0.075 (3)0.0118 (18)0.014 (2)0.009 (2)
C50.066 (3)0.032 (3)0.077 (4)0.007 (2)0.005 (3)0.000 (2)
C60.058 (3)0.032 (3)0.062 (3)0.003 (2)0.012 (2)0.003 (2)
N50.0369 (17)0.0322 (19)0.0400 (19)0.0020 (14)0.0016 (14)0.0025 (15)
C70.0349 (19)0.040 (2)0.041 (2)0.0049 (17)0.0032 (17)0.0070 (19)
N60.0450 (19)0.037 (2)0.049 (2)0.0069 (16)0.0016 (17)0.0136 (17)
C80.047 (2)0.034 (2)0.058 (3)0.0000 (19)0.005 (2)0.001 (2)
C90.045 (2)0.040 (3)0.043 (2)0.0000 (18)0.0010 (19)0.0013 (19)
N70.0411 (18)0.041 (2)0.0354 (19)0.0001 (15)0.0044 (15)0.0010 (15)
C100.039 (2)0.044 (3)0.036 (2)0.0044 (18)0.0012 (17)0.0027 (19)
N80.061 (2)0.055 (3)0.046 (2)0.004 (2)0.0139 (19)0.009 (2)
C110.074 (3)0.060 (4)0.042 (3)0.006 (3)0.020 (2)0.002 (2)
C120.059 (3)0.045 (3)0.048 (3)0.004 (2)0.010 (2)0.005 (2)
N90.051 (2)0.038 (2)0.038 (2)0.0023 (16)0.0038 (16)0.0031 (16)
C130.057 (3)0.056 (3)0.041 (2)0.007 (2)0.006 (2)0.005 (2)
N100.082 (3)0.074 (4)0.044 (2)0.013 (3)0.013 (2)0.010 (2)
C140.087 (4)0.059 (4)0.056 (3)0.018 (3)0.003 (3)0.018 (3)
C150.065 (3)0.045 (3)0.049 (3)0.002 (2)0.000 (2)0.008 (2)
N110.047 (2)0.047 (2)0.042 (2)0.0007 (17)0.0046 (16)0.0056 (18)
C160.057 (3)0.059 (3)0.035 (2)0.003 (2)0.007 (2)0.009 (2)
N120.069 (3)0.080 (4)0.043 (2)0.002 (3)0.013 (2)0.015 (2)
C170.069 (3)0.061 (4)0.058 (3)0.005 (3)0.001 (3)0.017 (3)
C180.057 (3)0.048 (3)0.052 (3)0.002 (2)0.001 (2)0.010 (2)
N130.0406 (18)0.037 (2)0.042 (2)0.0040 (15)0.0016 (15)0.0011 (16)
C190.039 (2)0.045 (3)0.048 (3)0.0065 (19)0.0028 (19)0.003 (2)
N140.048 (2)0.062 (3)0.059 (3)0.010 (2)0.0158 (19)0.007 (2)
C200.060 (3)0.051 (3)0.069 (4)0.011 (3)0.003 (3)0.006 (3)
C210.051 (3)0.039 (3)0.056 (3)0.004 (2)0.002 (2)0.001 (2)
N150.0411 (18)0.041 (2)0.047 (2)0.0057 (16)0.0054 (16)0.0005 (17)
C220.039 (2)0.049 (3)0.046 (3)0.002 (2)0.0083 (19)0.002 (2)
N160.050 (2)0.056 (3)0.064 (3)0.008 (2)0.016 (2)0.008 (2)
C230.060 (3)0.044 (3)0.080 (4)0.009 (2)0.007 (3)0.012 (3)
C240.058 (3)0.036 (3)0.061 (3)0.004 (2)0.003 (2)0.002 (2)
O10.0518 (19)0.054 (2)0.056 (2)0.0092 (15)0.0046 (16)0.0093 (16)
O20.056 (2)0.114 (4)0.068 (3)0.008 (2)0.013 (2)0.010 (2)
Cl10.0715 (10)0.1087 (15)0.0835 (12)0.0251 (10)0.0136 (9)0.0190 (11)
O30.067 (3)0.102 (4)0.119 (4)0.012 (3)0.028 (3)0.024 (3)
O40.266 (11)0.140 (8)0.354 (15)0.120 (8)0.114 (11)0.082 (9)
O50.116 (4)0.223 (9)0.107 (5)0.024 (5)0.053 (4)0.035 (5)
O60.088 (4)0.432 (17)0.159 (7)0.027 (7)0.001 (5)0.138 (9)
Cl20.0787 (9)0.0601 (9)0.0635 (8)0.0045 (7)0.0220 (7)0.0035 (7)
O70.161 (6)0.205 (8)0.158 (6)0.067 (6)0.058 (5)0.124 (6)
O80.259 (10)0.385 (16)0.094 (5)0.225 (11)0.034 (6)0.052 (7)
O90.171 (7)0.096 (5)0.223 (8)0.008 (4)0.143 (6)0.011 (5)
O100.278 (11)0.071 (4)0.324 (12)0.035 (5)0.228 (10)0.013 (6)
Cl30.0766 (12)0.1158 (18)0.1208 (18)0.0125 (11)0.0247 (11)0.0101 (15)
O110.252 (12)0.311 (18)0.310 (16)0.114 (12)0.134 (11)0.009 (13)
O120.080 (5)0.300 (14)0.46 (2)0.050 (7)0.047 (8)0.141 (13)
O130.249 (12)0.60 (3)0.095 (7)0.103 (14)0.065 (7)0.027 (11)
O140.350 (16)0.210 (12)0.222 (11)0.090 (11)0.054 (11)0.091 (9)
Cl4A0.0759 (18)0.0410 (15)0.0700 (18)0.0079 (12)0.0118 (14)0.0033 (12)
O15A0.123 (6)0.049 (4)0.070 (4)0.000 (4)0.011 (4)0.010 (3)
Cl4B0.077 (4)0.048 (3)0.117 (6)0.003 (2)0.014 (4)0.008 (3)
O15B0.126 (13)0.058 (9)0.172 (18)0.012 (9)0.000 (12)0.032 (11)
O160.148 (5)0.116 (5)0.106 (5)0.035 (4)0.003 (4)0.003 (4)
O170.140 (5)0.061 (3)0.138 (5)0.001 (3)0.020 (4)0.024 (3)
O180.160 (5)0.110 (5)0.091 (4)0.040 (4)0.013 (4)0.015 (4)
O190.164 (5)0.058 (3)0.126 (5)0.018 (3)0.081 (4)0.003 (3)
O200.138 (6)0.241 (10)0.130 (6)0.021 (6)0.080 (5)0.040 (6)
O210.122 (5)0.123 (5)0.107 (5)0.020 (4)0.059 (4)0.017 (4)
O220.128 (4)0.093 (4)0.103 (4)0.012 (3)0.008 (3)0.006 (3)
O230.064 (3)0.369 (14)0.211 (9)0.002 (5)0.003 (4)0.175 (9)
Geometric parameters (Å, º) top
Rh1—N72.045 (4)N10—H10N0.8600
Rh1—N12.049 (4)C14—C151.352 (8)
Rh1—N52.050 (4)C14—H140.9300
Rh1—N32.054 (4)C15—H150.9300
Rh1—O12.328 (3)N11—C161.329 (6)
Rh1—Rh22.6488 (6)N11—C181.373 (6)
Rh2—N132.048 (4)C16—N121.336 (7)
Rh2—N112.051 (4)N12—C171.347 (8)
Rh2—N92.057 (4)N12—H12N0.8600
Rh2—N152.061 (4)C17—C181.354 (8)
Rh2—O22.282 (4)C17—H170.9300
N1—C11.331 (6)C18—H180.9300
N1—C31.373 (6)N13—C191.332 (6)
C1—N21.337 (6)N13—C211.374 (6)
C1—C41.436 (7)C19—N141.335 (6)
N2—C21.357 (8)C19—C221.430 (7)
N2—H2N0.8600N14—C201.372 (7)
C2—C31.382 (7)N14—H14N0.8600
C2—H20.9300C20—C211.339 (7)
C3—H30.9300C20—H200.9300
N3—C41.325 (6)C21—H210.9300
N3—C61.371 (6)N15—C221.327 (6)
C4—N41.342 (6)N15—C241.372 (6)
N4—C51.348 (7)C22—N161.327 (6)
N4—H4N0.8600N16—C231.379 (7)
C5—C61.369 (7)N16—H16N0.8600
C5—H50.9300C23—C241.350 (8)
C6—H60.9300C23—H230.9300
N5—C71.325 (6)C24—H240.9300
N5—C91.359 (6)Cl1—O61.340 (7)
C7—N61.343 (6)Cl1—O41.395 (9)
C7—C101.432 (7)Cl1—O51.399 (6)
N6—C81.366 (6)Cl1—O31.409 (4)
N6—H6N0.8600Cl2—O101.336 (7)
C8—C91.345 (7)Cl2—O71.368 (6)
C8—H80.9300Cl2—O91.376 (6)
C9—H90.9300Cl2—O81.381 (7)
N7—C101.332 (6)Cl3—O121.273 (7)
N7—C121.379 (6)Cl3—O141.278 (9)
C10—N81.341 (6)Cl3—O131.330 (11)
N8—C111.359 (7)Cl3—O111.344 (12)
N8—H8N0.8600Cl4A—O171.360 (6)
C11—C121.360 (7)Cl4A—O181.367 (6)
C11—H110.9300Cl4A—O15A1.449 (8)
C12—H120.9300Cl4A—O161.532 (8)
N9—C131.330 (6)Cl4B—O161.173 (8)
N9—C151.364 (6)Cl4B—O15B1.34 (2)
C13—N101.334 (7)Cl4B—O181.529 (9)
C13—C161.440 (8)Cl4B—O171.574 (11)
N10—C141.370 (8)
O20···O112.790 (18)O18···O22ii2.770 (8)
O22···O12.744 (6)O23···O7ii3.070 (12)
O23···O22.678 (8)O21···O15Biii3.193 (18)
O19···O7i2.916 (9)O22···O12iv3.177 (14)
O19···O8i3.146 (11)O21···O4v3.291 (13)
O19···O5i3.018 (9)O23···O5v3.173 (12)
O20···O21i3.100 (10)O23···O4v3.281 (15)
O20···O8i3.131 (12)
N7—Rh1—N1173.08 (14)C15—N9—Rh2139.8 (4)
N7—Rh1—N579.53 (15)N9—C13—N10110.3 (5)
N1—Rh1—N5100.15 (15)N9—C13—C16116.2 (4)
N7—Rh1—N399.95 (15)N10—C13—C16133.5 (5)
N1—Rh1—N379.78 (15)C13—N10—C14107.8 (5)
N5—Rh1—N3175.18 (13)C13—N10—H10N126.1
N7—Rh1—O188.46 (14)C14—N10—H10N126.1
N1—Rh1—O184.62 (14)C15—C14—N10106.2 (5)
N5—Rh1—O186.72 (12)C15—C14—H14126.9
N3—Rh1—O188.48 (13)N10—C14—H14126.9
N7—Rh1—Rh293.23 (10)C14—C15—N9109.3 (5)
N1—Rh1—Rh293.69 (10)C14—C15—H15125.3
N5—Rh1—Rh291.67 (9)N9—C15—H15125.3
N3—Rh1—Rh293.14 (10)C16—N11—C18106.3 (4)
O1—Rh1—Rh2177.42 (10)C16—N11—Rh2113.5 (3)
N13—Rh2—N11174.14 (14)C18—N11—Rh2140.1 (4)
N13—Rh2—N999.67 (16)N11—C16—N12110.3 (5)
N11—Rh2—N979.56 (17)N11—C16—C13116.9 (4)
N13—Rh2—N1579.41 (16)N12—C16—C13132.8 (5)
N11—Rh2—N15100.95 (17)C16—N12—C17107.7 (5)
N9—Rh2—N15176.01 (14)C16—N12—H12N126.1
N13—Rh2—O287.62 (16)C17—N12—H12N126.1
N11—Rh2—O286.54 (16)N12—C17—C18107.6 (5)
N9—Rh2—O288.12 (16)N12—C17—H17126.2
N15—Rh2—O287.96 (16)C18—C17—H17126.2
N13—Rh2—Rh193.64 (9)C17—C18—N11108.1 (5)
N11—Rh2—Rh192.20 (10)C17—C18—H18126.0
N9—Rh2—Rh191.82 (10)N11—C18—H18126.0
N15—Rh2—Rh192.11 (10)C19—N13—C21105.5 (4)
O2—Rh2—Rh1178.73 (13)C19—N13—Rh2113.3 (3)
C1—N1—C3106.6 (4)C21—N13—Rh2140.5 (3)
C1—N1—Rh1113.2 (3)N13—C19—N14111.0 (5)
C3—N1—Rh1139.9 (3)N13—C19—C22117.0 (4)
N1—C1—N2110.3 (5)N14—C19—C22132.0 (5)
N1—C1—C4116.7 (4)C19—N14—C20107.1 (5)
N2—C1—C4132.9 (5)C19—N14—H14N126.5
C1—N2—C2108.6 (4)C20—N14—H14N126.5
C1—N2—H2N125.7C21—C20—N14106.9 (5)
C2—N2—H2N125.7C21—C20—H20126.5
N2—C2—C3106.1 (5)N14—C20—H20126.5
N2—C2—H2126.9C20—C21—N13109.5 (5)
C3—C2—H2126.9C20—C21—H21125.3
N1—C3—C2108.3 (5)N13—C21—H21125.3
N1—C3—H3125.9C22—N15—C24106.2 (4)
C2—C3—H3125.9C22—N15—Rh2113.4 (3)
C4—N3—C6106.4 (4)C24—N15—Rh2140.0 (4)
C4—N3—Rh1113.2 (3)N16—C22—N15111.2 (5)
C6—N3—Rh1140.2 (3)N16—C22—C19132.4 (5)
N3—C4—N4110.9 (4)N15—C22—C19116.4 (4)
N3—C4—C1116.8 (4)C22—N16—C23107.1 (5)
N4—C4—C1132.3 (5)C22—N16—H16N126.5
C4—N4—C5107.3 (4)C23—N16—H16N126.5
C4—N4—H4N126.3C24—C23—N16106.7 (5)
C5—N4—H4N126.3C24—C23—H23126.6
N4—C5—C6107.4 (5)N16—C23—H23126.6
N4—C5—H5126.3C23—C24—N15108.8 (5)
C6—C5—H5126.3C23—C24—H24125.6
C5—C6—N3108.0 (5)N15—C24—H24125.6
C5—C6—H6126.0O6—Cl1—O4109.8 (8)
N3—C6—H6126.0O6—Cl1—O5108.1 (6)
C7—N5—C9106.0 (4)O4—Cl1—O5108.5 (6)
C7—N5—Rh1113.5 (3)O6—Cl1—O3111.1 (4)
C9—N5—Rh1140.3 (3)O4—Cl1—O3106.6 (5)
N5—C7—N6110.5 (4)O5—Cl1—O3112.6 (4)
N5—C7—C10116.8 (4)O10—Cl2—O7110.8 (7)
N6—C7—C10132.7 (4)O10—Cl2—O9104.2 (4)
C7—N6—C8107.3 (4)O7—Cl2—O9117.5 (5)
C7—N6—H6N126.3O10—Cl2—O8109.8 (8)
C8—N6—H6N126.3O7—Cl2—O8104.3 (5)
C9—C8—N6106.3 (4)O9—Cl2—O8110.2 (6)
C9—C8—H8126.9O12—Cl3—O14120.9 (8)
N6—C8—H8126.9O12—Cl3—O13102.8 (9)
C8—C9—N5110.0 (4)O14—Cl3—O13113.1 (9)
C8—C9—H9125.0O12—Cl3—O11113.8 (10)
N5—C9—H9125.0O14—Cl3—O11100.8 (9)
C10—N7—C12106.9 (4)O13—Cl3—O11104.6 (10)
C10—N7—Rh1113.7 (3)O17—Cl4A—O18118.4 (4)
C12—N7—Rh1138.9 (3)O17—Cl4A—O15A107.6 (5)
N7—C10—N8110.2 (4)O18—Cl4A—O15A106.4 (5)
N7—C10—C7116.2 (4)O17—Cl4A—O16108.2 (5)
N8—C10—C7133.5 (4)O18—Cl4A—O16109.1 (4)
C10—N8—C11107.5 (4)O15A—Cl4A—O16106.6 (4)
C10—N8—H8N126.2O16—Cl4B—O15B117.3 (12)
C11—N8—H8N126.2O16—Cl4B—O18121.4 (7)
N8—C11—C12107.8 (5)O15B—Cl4B—O1899.1 (9)
N8—C11—H11126.1O16—Cl4B—O17116.4 (7)
C12—C11—H11126.1O15B—Cl4B—O17100.8 (9)
C11—C12—N7107.6 (5)O18—Cl4B—O1798.0 (6)
C11—C12—H12126.2Cl4B—O16—Cl4A35.2 (5)
N7—C12—H12126.2Cl4A—O17—Cl4B34.2 (3)
C13—N9—C15106.3 (4)Cl4A—O18—Cl4B35.1 (3)
C13—N9—Rh2113.6 (3)
N7—Rh1—Rh2—N1342.27 (15)C12—N7—C10—C7177.6 (4)
N1—Rh1—Rh2—N13137.62 (15)Rh1—N7—C10—C74.7 (5)
N5—Rh1—Rh2—N1337.33 (15)N5—C7—C10—N71.2 (5)
N3—Rh1—Rh2—N13142.43 (15)N6—C7—C10—N7179.8 (4)
O1—Rh1—Rh2—N1389 (2)N5—C7—C10—N8176.7 (4)
N7—Rh1—Rh2—N11138.30 (16)N6—C7—C10—N82.0 (8)
N1—Rh1—Rh2—N1141.81 (16)N7—C10—N8—C110.9 (5)
N5—Rh1—Rh2—N11142.10 (16)C7—C10—N8—C11177.0 (5)
N3—Rh1—Rh2—N1138.13 (16)C10—N8—C11—C120.7 (6)
O1—Rh1—Rh2—N1191 (2)N8—C11—C12—N70.2 (6)
N7—Rh1—Rh2—N9142.09 (16)C10—N7—C12—C110.3 (6)
N1—Rh1—Rh2—N937.81 (15)Rh1—N7—C12—C11170.3 (4)
N5—Rh1—Rh2—N962.48 (15)N13—Rh2—N9—C13169.7 (3)
N3—Rh1—Rh2—N9117.75 (15)N11—Rh2—N9—C134.4 (3)
O1—Rh1—Rh2—N911 (2)N15—Rh2—N9—C1393 (2)
N7—Rh1—Rh2—N1537.25 (16)O2—Rh2—N9—C1382.4 (3)
N1—Rh1—Rh2—N15142.86 (15)Rh1—Rh2—N9—C1396.3 (3)
N5—Rh1—Rh2—N15116.85 (15)N13—Rh2—N9—C152.8 (5)
N3—Rh1—Rh2—N1562.91 (15)N11—Rh2—N9—C15176.9 (5)
O1—Rh1—Rh2—N15168 (2)N15—Rh2—N9—C1579 (2)
N7—Rh1—Rh2—O2131 (6)O2—Rh2—N9—C1590.1 (5)
N1—Rh1—Rh2—O249 (6)Rh1—Rh2—N9—C1591.2 (5)
N5—Rh1—Rh2—O2150 (6)C15—N9—C13—N101.2 (6)
N3—Rh1—Rh2—O231 (6)Rh2—N9—C13—N10176.1 (3)
O1—Rh1—Rh2—O298 (6)C15—N9—C13—C16179.7 (4)
N7—Rh1—N1—C183.3 (13)Rh2—N9—C13—C164.7 (5)
N5—Rh1—N1—C1170.0 (3)N9—C13—N10—C140.8 (6)
N3—Rh1—N1—C15.1 (3)C16—C13—N10—C14179.8 (5)
O1—Rh1—N1—C184.3 (3)C13—N10—C14—C150.1 (6)
Rh2—Rh1—N1—C197.6 (3)N10—C14—C15—N90.6 (6)
N7—Rh1—N1—C389.2 (13)C13—N9—C15—C141.1 (6)
N5—Rh1—N1—C32.5 (5)Rh2—N9—C15—C14174.0 (4)
N3—Rh1—N1—C3177.6 (5)N13—Rh2—N11—C1679.6 (16)
O1—Rh1—N1—C388.2 (5)N9—Rh2—N11—C163.4 (3)
Rh2—Rh1—N1—C389.9 (5)N15—Rh2—N11—C16172.5 (3)
C3—N1—C1—N20.3 (6)O2—Rh2—N11—C1685.3 (3)
Rh1—N1—C1—N2174.6 (3)Rh1—Rh2—N11—C1694.9 (3)
C3—N1—C1—C4179.1 (4)N13—Rh2—N11—C1895.4 (16)
Rh1—N1—C1—C44.1 (5)N9—Rh2—N11—C18178.4 (5)
N1—C1—N2—C20.5 (6)N15—Rh2—N11—C182.5 (5)
C4—C1—N2—C2179.0 (5)O2—Rh2—N11—C1889.7 (5)
C1—N2—C2—C30.5 (7)Rh1—Rh2—N11—C1890.1 (5)
C1—N1—C3—C20.0 (6)C18—N11—C16—N121.2 (6)
Rh1—N1—C3—C2172.8 (4)Rh2—N11—C16—N12177.9 (3)
N2—C2—C3—N10.3 (7)C18—N11—C16—C13178.7 (4)
N7—Rh1—N3—C4167.6 (3)Rh2—N11—C16—C132.0 (5)
N1—Rh1—N3—C45.4 (3)N9—C13—C16—N111.8 (7)
N5—Rh1—N3—C484.2 (18)N10—C13—C16—N11179.3 (5)
O1—Rh1—N3—C479.4 (3)N9—C13—C16—N12178.3 (5)
Rh2—Rh1—N3—C498.6 (3)N10—C13—C16—N120.7 (10)
N7—Rh1—N3—C66.8 (5)N11—C16—N12—C171.0 (6)
N1—Rh1—N3—C6179.7 (5)C13—C16—N12—C17178.9 (5)
N5—Rh1—N3—C690.1 (18)C16—N12—C17—C180.3 (6)
O1—Rh1—N3—C694.9 (5)N12—C17—C18—N110.4 (6)
Rh2—Rh1—N3—C687.1 (5)C16—N11—C18—C171.0 (5)
C6—N3—C4—N40.6 (5)Rh2—N11—C18—C17176.2 (4)
Rh1—N3—C4—N4176.8 (3)N11—Rh2—N13—C1988.5 (16)
C6—N3—C4—C1178.9 (4)N9—Rh2—N13—C19170.5 (3)
Rh1—N3—C4—C14.9 (5)N15—Rh2—N13—C195.5 (3)
N1—C1—C4—N30.5 (6)O2—Rh2—N13—C1982.8 (3)
N2—C1—C4—N3178.9 (5)Rh1—Rh2—N13—C1997.0 (3)
N1—C1—C4—N4178.4 (5)N11—Rh2—N13—C2180.3 (17)
N2—C1—C4—N43.2 (9)N9—Rh2—N13—C211.7 (5)
N3—C4—N4—C50.2 (6)N15—Rh2—N13—C21174.4 (5)
C1—C4—N4—C5178.1 (5)O2—Rh2—N13—C2186.0 (5)
C4—N4—C5—C60.3 (6)Rh1—Rh2—N13—C2194.2 (5)
N4—C5—C6—N30.6 (6)C21—N13—C19—N140.8 (5)
C4—N3—C6—C50.7 (5)Rh2—N13—C19—N14173.4 (3)
Rh1—N3—C6—C5175.3 (4)C21—N13—C19—C22177.3 (4)
N7—Rh1—N5—C74.2 (3)Rh2—N13—C19—C224.7 (5)
N1—Rh1—N5—C7168.8 (3)N13—C19—N14—C200.5 (5)
N3—Rh1—N5—C780.1 (18)C22—C19—N14—C20177.2 (5)
O1—Rh1—N5—C784.9 (3)C19—N14—C20—C210.0 (6)
Rh2—Rh1—N5—C797.1 (3)N14—C20—C21—N130.5 (6)
N7—Rh1—N5—C9177.6 (4)C19—N13—C21—C200.8 (5)
N1—Rh1—N5—C94.6 (4)Rh2—N13—C21—C20170.2 (4)
N3—Rh1—N5—C993.3 (18)N13—Rh2—N15—C225.7 (3)
O1—Rh1—N5—C988.5 (4)N11—Rh2—N15—C22168.4 (3)
Rh2—Rh1—N5—C989.5 (4)N9—Rh2—N15—C2271 (2)
C9—N5—C7—N60.3 (4)O2—Rh2—N15—C2282.3 (3)
Rh1—N5—C7—N6176.0 (2)Rh1—Rh2—N15—C2299.0 (3)
C9—N5—C7—C10178.6 (3)N13—Rh2—N15—C24177.1 (5)
Rh1—N5—C7—C103.0 (4)N11—Rh2—N15—C243.1 (5)
N5—C7—N6—C80.5 (5)N9—Rh2—N15—C24100 (2)
C10—C7—N6—C8178.2 (4)O2—Rh2—N15—C2489.2 (5)
C7—N6—C8—C90.4 (5)Rh1—Rh2—N15—C2489.6 (5)
N6—C8—C9—N50.2 (5)C24—N15—C22—N161.4 (5)
C7—N5—C9—C80.1 (5)Rh2—N15—C22—N16175.7 (3)
Rh1—N5—C9—C8173.8 (3)C24—N15—C22—C19179.3 (4)
N1—Rh1—N7—C1083.2 (13)Rh2—N15—C22—C195.0 (5)
N5—Rh1—N7—C104.8 (3)N13—C19—C22—N16179.4 (5)
N3—Rh1—N7—C10170.3 (3)N14—C19—C22—N163.0 (9)
O1—Rh1—N7—C1082.1 (3)N13—C19—C22—N150.2 (6)
Rh2—Rh1—N7—C1095.9 (3)N14—C19—C22—N15177.8 (5)
N1—Rh1—N7—C1286.3 (13)N15—C22—N16—C231.1 (6)
N5—Rh1—N7—C12174.3 (5)C19—C22—N16—C23179.7 (5)
N3—Rh1—N7—C120.8 (5)C22—N16—C23—C240.4 (6)
O1—Rh1—N7—C1287.4 (5)N16—C23—C24—N150.4 (6)
Rh2—Rh1—N7—C1294.6 (5)C22—N15—C24—C231.1 (6)
C12—N7—C10—N80.8 (5)Rh2—N15—C24—C23172.9 (4)
Rh1—N7—C10—N8173.6 (3)
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1/2, y+1/2, z1/2; (iv) x+1/2, y1/2, z+3/2; (v) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O190.862.052.829 (7)151
N4—H4N···O190.862.273.013 (7)145
N4—H4N···O10vi0.862.523.104 (8)126
N6—H6N···O30.862.273.038 (7)149
N6—H6N···O1vii0.862.523.128 (5)128
N8—H8N···O30.862.222.991 (7)150
N8—H8N···O80.862.583.107 (8)121
N10—H10N···O110.862.183.014 (13)163
N12—H12N···O200.861.972.819 (8)167
N14—H14N···O210.862.112.884 (8)150
N16—H16N···O210.862.182.949 (8)148
Symmetry codes: (vi) x+1, y, z+1; (vii) x+1, y+1, z+1.
(III) top
Crystal data top
C26H32N16O2Rh2·4(ClO4)Dx = 1.890 Mg m3
Mr = 1204.30Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, PbcnCell parameters from 9792 reflections
a = 20.119 (5) Åθ = 3.0–27.5°
b = 16.115 (4) ŵ = 1.13 mm1
c = 13.055 (3) ÅT = 296 K
V = 4232.9 (17) Å3Prismatic, green
Z = 40.42 × 0.35 × 0.32 mm
F(000) = 2408
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
4835 independent reflections
Radiation source: rotating-anode X-ray tube4243 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = 2625
Absorption correction: numerical
NUMABS (Higashi, 1999)
k = 2020
Tmin = 0.740, Tmax = 0.803l = 1416
30878 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.126H atoms treated by a mixture of independent and constrained refinement
S = 1.16 w = 1/[σ2(Fo2) + (0.0552P)2 + 4.7874P]
where P = (Fo2 + 2Fc2)/3
4838 reflections(Δ/σ)max = 0.001
302 parametersΔρmax = 1.04 e Å3
1 restraintΔρmin = 0.61 e Å3
Crystal data top
C26H32N16O2Rh2·4(ClO4)V = 4232.9 (17) Å3
Mr = 1204.30Z = 4
Orthorhombic, PbcnMo Kα radiation
a = 20.119 (5) ŵ = 1.13 mm1
b = 16.115 (4) ÅT = 296 K
c = 13.055 (3) Å0.42 × 0.35 × 0.32 mm
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
4835 independent reflections
Absorption correction: numerical
NUMABS (Higashi, 1999)
4243 reflections with I > 2σ(I)
Tmin = 0.740, Tmax = 0.803Rint = 0.033
30878 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0501 restraint
wR(F2) = 0.126H atoms treated by a mixture of independent and constrained refinement
S = 1.16Δρmax = 1.04 e Å3
4838 reflectionsΔρmin = 0.61 e Å3
302 parameters
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 not 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
xyzUiso*/Ueq
Rh10.497490 (11)0.271040 (16)0.64762 (2)0.03020 (11)
N10.59303 (14)0.31328 (19)0.6312 (2)0.0338 (6)
C10.63709 (18)0.2521 (2)0.6151 (3)0.0380 (8)
N20.69761 (15)0.2844 (2)0.5973 (3)0.0477 (9)
H2N0.73350.25690.58620.057*
C20.6918 (2)0.3688 (3)0.6000 (4)0.0503 (10)
H20.72560.40730.58980.060*
C30.62670 (19)0.3860 (3)0.6206 (3)0.0417 (9)
H30.60840.43870.62630.050*
N30.54734 (14)0.16006 (18)0.6369 (2)0.0357 (7)
C40.61244 (18)0.1688 (2)0.6198 (3)0.0386 (8)
N40.64145 (16)0.0952 (2)0.6080 (3)0.0475 (8)
H4N0.68300.08650.59690.057*
C50.5934 (2)0.0364 (3)0.6169 (4)0.0520 (10)
H50.59920.02070.61160.062*
C60.5351 (2)0.0768 (2)0.6348 (3)0.0432 (9)
H60.49380.05180.64400.052*
N50.44682 (15)0.38132 (19)0.6460 (2)0.0353 (7)
C70.38098 (18)0.3726 (2)0.6400 (3)0.0369 (8)
N60.35148 (16)0.4461 (2)0.6299 (3)0.0471 (8)
H6N0.30940.45480.62540.057*
C80.4001 (2)0.5049 (3)0.6282 (4)0.0504 (10)
H80.39400.56190.62160.061*
C90.4589 (2)0.4646 (2)0.6377 (3)0.0429 (9)
H90.50060.48940.63850.052*
N70.40188 (15)0.22891 (19)0.6486 (2)0.0353 (7)
C100.35631 (18)0.2885 (3)0.6435 (3)0.0388 (8)
N80.29523 (16)0.2558 (2)0.6397 (3)0.0453 (8)
H8N0.25840.28290.63770.054*
C110.30196 (19)0.1716 (3)0.6396 (3)0.0483 (10)
H110.26780.13270.63650.058*
C120.36819 (19)0.1555 (3)0.6448 (3)0.0432 (9)
H120.38740.10300.64570.052*
O10.49253 (15)0.2775 (2)0.4713 (3)0.0576 (8)
H10.4653 (19)0.313 (2)0.461 (4)0.069*
C130.4931 (5)0.2148 (6)0.4038 (6)0.161 (5)
H130.51250.16660.43510.242*
H13A0.51890.23040.34490.242*
H13B0.44840.20240.38300.242*
Cl10.83630 (5)0.13164 (7)0.64406 (9)0.0534 (3)
O20.8199 (3)0.1982 (4)0.5815 (4)0.142 (3)
O30.7906 (2)0.0702 (4)0.6377 (7)0.189 (4)
O40.89949 (15)0.1003 (2)0.6126 (3)0.0670 (9)
O50.8381 (3)0.1616 (4)0.7444 (3)0.128 (2)
Cl20.16651 (6)0.41641 (8)0.65875 (11)0.0644 (4)
O60.2100 (2)0.4742 (3)0.6073 (5)0.133 (2)
O70.17426 (18)0.3388 (2)0.6079 (3)0.0777 (11)
O80.1864 (3)0.4092 (5)0.7603 (4)0.161 (3)
O90.10097 (16)0.4456 (2)0.6486 (3)0.0785 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.02584 (16)0.03121 (17)0.03355 (18)0.00317 (10)0.00061 (10)0.00026 (11)
N10.0301 (14)0.0357 (15)0.0355 (17)0.0002 (12)0.0006 (12)0.0013 (13)
C10.0297 (17)0.044 (2)0.040 (2)0.0057 (15)0.0032 (16)0.0006 (17)
N20.0302 (16)0.058 (2)0.055 (2)0.0031 (14)0.0065 (15)0.0012 (17)
C20.044 (2)0.053 (2)0.054 (3)0.0092 (19)0.0025 (19)0.003 (2)
C30.0382 (19)0.042 (2)0.045 (2)0.0005 (16)0.0004 (17)0.0030 (17)
N30.0319 (15)0.0367 (15)0.0386 (18)0.0044 (12)0.0018 (12)0.0008 (13)
C40.0352 (18)0.042 (2)0.039 (2)0.0054 (16)0.0045 (15)0.0017 (16)
N40.0411 (17)0.0464 (19)0.055 (2)0.0148 (15)0.0071 (16)0.0017 (16)
C50.056 (2)0.040 (2)0.060 (3)0.0080 (19)0.004 (2)0.000 (2)
C60.045 (2)0.0354 (19)0.049 (2)0.0029 (16)0.0010 (17)0.0003 (17)
N50.0334 (15)0.0373 (16)0.0352 (17)0.0059 (13)0.0016 (12)0.0008 (13)
C70.0355 (18)0.0396 (19)0.036 (2)0.0081 (15)0.0000 (15)0.0037 (16)
N60.0407 (17)0.0470 (19)0.054 (2)0.0168 (15)0.0052 (15)0.0008 (16)
C80.057 (2)0.035 (2)0.060 (3)0.0108 (18)0.007 (2)0.0002 (19)
C90.046 (2)0.0375 (19)0.046 (2)0.0004 (17)0.0039 (17)0.0014 (17)
N70.0295 (15)0.0398 (17)0.0368 (18)0.0027 (12)0.0029 (12)0.0020 (13)
C100.0276 (17)0.052 (2)0.036 (2)0.0052 (16)0.0011 (14)0.0002 (17)
N80.0265 (15)0.0531 (19)0.056 (2)0.0049 (14)0.0023 (14)0.0023 (16)
C110.0346 (19)0.052 (2)0.059 (3)0.0052 (17)0.0038 (17)0.001 (2)
C120.0386 (19)0.0384 (19)0.053 (3)0.0019 (16)0.0006 (17)0.0070 (17)
O10.0607 (19)0.069 (2)0.0430 (19)0.0178 (15)0.0112 (15)0.0015 (16)
C130.244 (13)0.168 (9)0.071 (5)0.132 (8)0.051 (6)0.050 (5)
Cl10.0412 (5)0.0613 (6)0.0577 (7)0.0131 (5)0.0093 (5)0.0090 (5)
O20.142 (4)0.179 (5)0.105 (4)0.120 (4)0.052 (3)0.074 (4)
O30.062 (3)0.129 (5)0.375 (12)0.032 (3)0.062 (4)0.073 (5)
O40.0462 (17)0.063 (2)0.092 (3)0.0149 (15)0.0173 (17)0.0094 (18)
O50.122 (4)0.193 (6)0.068 (3)0.064 (4)0.005 (3)0.019 (3)
Cl20.0445 (6)0.0644 (7)0.0841 (9)0.0197 (5)0.0173 (5)0.0218 (6)
O60.059 (2)0.074 (3)0.265 (7)0.006 (2)0.011 (3)0.000 (4)
O70.070 (2)0.066 (2)0.097 (3)0.0290 (18)0.018 (2)0.018 (2)
O80.166 (5)0.220 (7)0.096 (4)0.102 (5)0.070 (4)0.064 (4)
O90.0445 (17)0.078 (2)0.114 (3)0.0212 (17)0.0125 (18)0.020 (2)
Geometric parameters (Å, º) top
Rh1—N72.040 (3)N6—C81.362 (6)
Rh1—N52.049 (3)N6—H6N0.8600
Rh1—N12.050 (3)C8—C91.357 (6)
Rh1—N32.055 (3)C8—H80.9300
Rh1—O12.307 (4)C9—H90.9300
Rh1—Rh1i2.6752 (9)N7—C101.330 (5)
N1—C11.343 (5)N7—C121.365 (5)
N1—C31.360 (5)C10—N81.339 (5)
C1—N21.345 (5)N8—C111.363 (5)
C1—C41.432 (5)N8—H8N0.8600
N2—C21.366 (5)C11—C121.359 (5)
N2—H2N0.8600C11—H110.9300
C2—C31.364 (5)C12—H120.9300
C2—H20.9300O1—C131.341 (8)
C3—H30.9300O1—H10.805 (19)
N3—C41.336 (5)C13—H130.9600
N3—C61.365 (5)C13—H13A0.9600
C4—N41.331 (5)C13—H13B0.9600
N4—C51.359 (5)Cl1—O31.354 (5)
N4—H4N0.8600Cl1—O21.389 (4)
C5—C61.362 (6)Cl1—O51.396 (5)
C5—H50.9300Cl1—O41.428 (3)
C6—H60.9300Cl2—O81.389 (5)
N5—C71.334 (5)Cl2—O91.406 (3)
N5—C91.368 (5)Cl2—O71.424 (4)
C7—N61.330 (5)Cl2—O61.443 (5)
C7—C101.444 (6)
N7—Rh1—N579.61 (12)N6—C7—N5110.8 (3)
N7—Rh1—N1174.38 (12)N6—C7—C10133.2 (3)
N5—Rh1—N1100.22 (12)N5—C7—C10116.0 (3)
N7—Rh1—N399.84 (12)C7—N6—C8107.5 (3)
N5—Rh1—N3175.47 (12)C7—N6—H6N126.2
N1—Rh1—N379.88 (12)C8—N6—H6N126.2
N7—Rh1—O188.90 (12)C9—C8—N6106.9 (4)
N5—Rh1—O185.94 (11)C9—C8—H8126.5
N1—Rh1—O185.49 (12)N6—C8—H8126.5
N3—Rh1—O189.56 (12)C8—C9—N5108.8 (4)
N7—Rh1—Rh1i91.67 (9)C8—C9—H9125.6
N5—Rh1—Rh1i91.66 (8)N5—C9—H9125.6
N1—Rh1—Rh1i93.95 (9)C10—N7—C12106.4 (3)
N3—Rh1—Rh1i92.85 (9)C10—N7—Rh1114.2 (3)
O1—Rh1—Rh1i177.39 (8)C12—N7—Rh1139.2 (3)
C1—N1—C3106.7 (3)N7—C10—N8110.5 (4)
C1—N1—Rh1113.0 (2)N7—C10—C7116.3 (3)
C3—N1—Rh1139.8 (3)N8—C10—C7133.2 (4)
N1—C1—N2109.9 (3)C10—N8—C11107.6 (3)
N1—C1—C4116.9 (3)C10—N8—H8N126.2
N2—C1—C4133.2 (3)C11—N8—H8N126.2
C1—N2—C2107.7 (3)C12—C11—N8106.7 (4)
C1—N2—H2N126.2C12—C11—H11126.6
C2—N2—H2N126.2N8—C11—H11126.6
C3—C2—N2106.8 (4)C11—C12—N7108.8 (4)
C3—C2—H2126.6C11—C12—H12125.6
N2—C2—H2126.6N7—C12—H12125.6
N1—C3—C2108.9 (4)C13—O1—Rh1128.4 (5)
N1—C3—H3125.6C13—O1—H1116 (4)
C2—C3—H3125.6Rh1—O1—H1103 (4)
C4—N3—C6106.1 (3)O1—C13—H13109.5
C4—N3—Rh1113.4 (2)O1—C13—H13A109.5
C6—N3—Rh1140.2 (3)H13—C13—H13A109.5
N4—C4—N3110.8 (3)O1—C13—H13B109.5
N4—C4—C1132.7 (3)H13—C13—H13B109.5
N3—C4—C1116.5 (3)H13A—C13—H13B109.5
C4—N4—C5107.4 (3)O3—Cl1—O2111.6 (5)
C4—N4—H4N126.3O3—Cl1—O5109.1 (4)
C5—N4—H4N126.3O2—Cl1—O5106.9 (4)
N4—C5—C6107.1 (4)O3—Cl1—O4109.1 (3)
N4—C5—H5126.4O2—Cl1—O4108.4 (2)
C6—C5—H5126.4O5—Cl1—O4111.6 (3)
C5—C6—N3108.5 (4)O8—Cl2—O9112.8 (3)
C5—C6—H6125.7O8—Cl2—O7109.9 (3)
N3—C6—H6125.7O9—Cl2—O7110.6 (2)
C7—N5—C9105.9 (3)O8—Cl2—O6108.8 (4)
C7—N5—Rh1113.8 (2)O9—Cl2—O6108.0 (3)
C9—N5—Rh1139.7 (3)O7—Cl2—O6106.5 (3)
N1—Rh1—Rh1i—N5i40.76 (12)N3—Rh1—N5—C7
N3—Rh1—Rh1i—N7i41.15 (12)O1—Rh1—N5—C7
N7—Rh1—N1—C1Rh1—Rh1i—N5—C7
N5—Rh1—N1—C1N7—Rh1—N5—C9
N3—Rh1—N1—C1N1—Rh1—N5—C9
O1—Rh1—N1—C1N3—Rh1—N5—C9
Rh1—Rh1i—N1—C1O1—Rh1—N5—C9
N7—Rh1—N1—C3Rh1—Rh1i—N5—C9
N5—Rh1—N1—C3C9—N5—C7—N6
N3—Rh1—N1—C3Rh1—N5—C7—N6
O1—Rh1—N1—C3C9—N5—C7—C10
Rh1—Rh1i—N1—C3Rh1—N5—C7—C10
C3—N1—C1—N2N5—C7—N6—C8
Rh1—N1—C1—N2C10—C7—N6—C8
C3—N1—C1—C4C7—N6—C8—C9
Rh1—N1—C1—C4N6—C8—C9—N5
N1—C1—N2—C2C7—N5—C9—C8
C4—C1—N2—C2Rh1—N5—C9—C8
C1—N2—C2—C3N5—Rh1—N7—C10
C1—N1—C3—C2N1—Rh1—N7—C10
Rh1—N1—C3—C2N3—Rh1—N7—C10
N2—C2—C3—N1O1—Rh1—N7—C10
N7—Rh1—N3—C4Rh1—Rh1i—N7—C10
N5—Rh1—N3—C4N5—Rh1—N7—C12
N1—Rh1—N3—C4N1—Rh1—N7—C12
O1—Rh1—N3—C4N3—Rh1—N7—C12
Rh1—Rh1i—N3—C4O1—Rh1—N7—C12
N7—Rh1—N3—C6Rh1—Rh1i—N7—C12
N5—Rh1—N3—C6C12—N7—C10—N8
N1—Rh1—N3—C6Rh1—N7—C10—N8
O1—Rh1—N3—C6C12—N7—C10—C7
Rh1—Rh1i—N3—C6Rh1—N7—C10—C7
C6—N3—C4—N4N6—C7—C10—N7
Rh1—N3—C4—N4N5—C7—C10—N7
C6—N3—C4—C1N6—C7—C10—N8
Rh1—N3—C4—C1N5—C7—C10—N8
N1—C1—C4—N4N7—C10—N8—C11
N2—C1—C4—N4C7—C10—N8—C11
N1—C1—C4—N3C10—N8—C11—C12
N2—C1—C4—N3N8—C11—C12—N7
N3—C4—N4—C5C10—N7—C12—C11
C1—C4—N4—C5Rh1—N7—C12—C11
C4—N4—C5—C6N7—Rh1—O1—C13
N4—C5—C6—N3N5—Rh1—O1—C13
C4—N3—C6—C5N1—Rh1—O1—C13
Rh1—N3—C6—C5N3—Rh1—O1—C13
N7—Rh1—N5—C7Rh1—Rh1i—O1—C13
N1—Rh1—N5—C7
Symmetry code: (i) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O20.861.982.833 (5)172
N4—H4N···O30.862.253.053 (6)156
N6—H6N···O60.862.042.897 (5)177
N8—H8N···O70.861.962.808 (5)170
O1—H1···O4ii0.81 (2)2.15 (2)2.929 (4)163 (5)
Symmetry code: (ii) x1/2, y+1/2, z+1.
(IV) top
Crystal data top
C30H38N18O2Rh2·4(BF4)F(000) = 2456
Mr = 1235.84Dx = 1.754 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
a = 16.073 (10) ÅCell parameters from 4208 reflections
b = 19.104 (11) Åθ = 3.0–27.5°
c = 16.399 (10) ŵ = 0.82 mm1
β = 111.673 (6)°T = 296 K
V = 4679 (5) Å3Prismatic, green
Z = 40.47 × 0.38 × 0.23 mm
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
5356 independent reflections
Radiation source: rotating-anode X-ray tube3475 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.056
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.0°
ω scansh = 2020
Absorption correction: numerical
NUMABS (Higashi, 1999)
k = 2224
Tmin = 0.765, Tmax = 0.891l = 2021
17721 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.213H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.1143P)2 + 8.0854P]
where P = (Fo2 + 2Fc2)/3
5356 reflections(Δ/σ)max < 0.001
392 parametersΔρmax = 2.60 e Å3
474 restraintsΔρmin = 0.94 e Å3
Crystal data top
C30H38N18O2Rh2·4(BF4)V = 4679 (5) Å3
Mr = 1235.84Z = 4
Monoclinic, C2/cMo Kα radiation
a = 16.073 (10) ŵ = 0.82 mm1
b = 19.104 (11) ÅT = 296 K
c = 16.399 (10) Å0.47 × 0.38 × 0.23 mm
β = 111.673 (6)°
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
5356 independent reflections
Absorption correction: numerical
NUMABS (Higashi, 1999)
3475 reflections with I > 2σ(I)
Tmin = 0.765, Tmax = 0.891Rint = 0.056
17721 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.066474 restraints
wR(F2) = 0.213H-atom parameters constrained
S = 1.05Δρmax = 2.60 e Å3
5356 reflectionsΔρmin = 0.94 e Å3
392 parameters
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 not 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
xyzUiso*/UeqOcc. (<1)
Rh10.41335 (3)0.249529 (18)0.23305 (3)0.03572 (19)
N10.4147 (3)0.1473 (2)0.2727 (3)0.0445 (10)
C10.3907 (4)0.1019 (3)0.2065 (4)0.0484 (13)
N20.3880 (4)0.0366 (3)0.2348 (4)0.0600 (14)
H2N0.37390.00060.20310.072*
C20.4115 (5)0.0404 (3)0.3226 (4)0.0667 (18)
H20.41630.00310.36050.080*
C30.4269 (4)0.1089 (3)0.3455 (4)0.0547 (15)
H30.44320.12650.40220.066*
N30.3833 (3)0.1988 (2)0.1155 (3)0.0461 (10)
C40.3711 (4)0.1304 (3)0.1198 (4)0.0491 (13)
N40.3405 (3)0.1017 (3)0.0403 (3)0.0596 (13)
H4N0.32810.05820.02810.071*
C50.3327 (4)0.1545 (4)0.0182 (4)0.0645 (17)
H50.31310.15020.07890.077*
C60.3589 (4)0.2139 (3)0.0285 (4)0.0576 (15)
H60.36010.25810.00520.069*
N50.4278 (3)0.2999 (2)0.3473 (3)0.0448 (10)
C70.4072 (4)0.3678 (3)0.3355 (4)0.0482 (13)
N60.4012 (4)0.3952 (3)0.4078 (3)0.0696 (16)
H6N0.38860.43800.41480.084*
C80.4183 (5)0.3433 (4)0.4682 (4)0.075 (2)
H80.41970.34760.52520.090*
C90.4330 (4)0.2843 (3)0.4305 (4)0.0551 (14)
H90.44470.24040.45660.066*
N70.4008 (3)0.3510 (2)0.1913 (3)0.0442 (10)
C100.3940 (4)0.3959 (3)0.2500 (4)0.0494 (13)
N80.3768 (5)0.4606 (3)0.2165 (4)0.0656 (15)
H8N0.36950.49760.24310.079*
C110.3732 (5)0.4568 (3)0.1329 (4)0.0699 (19)
H110.36250.49380.09350.084*
C120.3880 (4)0.3886 (3)0.1169 (4)0.0517 (14)
H120.38920.37100.06450.062*
O10.2648 (3)0.2572 (2)0.2061 (3)0.0508 (11)
C130.2404 (4)0.2318 (4)0.2615 (5)0.0620 (17)
H130.27940.20130.30200.074*
N90.1626 (4)0.2445 (3)0.2685 (5)0.0694 (18)
C140.1026 (7)0.2945 (7)0.2105 (7)0.133 (5)
H140.13530.33580.20740.200*
H14A0.05670.30660.23240.200*
H14B0.07560.27450.15300.200*
C150.1370 (6)0.2101 (6)0.3350 (6)0.102 (3)
H150.17930.17380.36280.154*
H15A0.07840.19000.30790.154*
H15B0.13630.24380.37820.154*
B10.3728 (6)0.5813 (4)0.3763 (5)0.084 (2)
F10.3661 (4)0.6447 (2)0.4079 (3)0.119 (2)
F2A0.3234 (11)0.5794 (7)0.2867 (6)0.097 (5)0.54 (3)
F3A0.4522 (8)0.5549 (8)0.3920 (12)0.135 (6)0.54 (3)
F4A0.3269 (15)0.5346 (6)0.4113 (12)0.135 (6)0.54 (3)
F2B0.3065 (11)0.5591 (12)0.3080 (13)0.138 (8)0.46 (3)
F3B0.4468 (12)0.5868 (13)0.3499 (17)0.162 (8)0.46 (3)
F4B0.399 (3)0.5367 (7)0.4449 (9)0.159 (10)0.46 (3)
B2A0.3488 (12)0.0920 (9)0.0443 (9)0.116 (6)0.421 (17)
B2B0.3638 (10)0.0916 (7)0.0493 (8)0.118 (5)0.579 (17)
F50.3608 (7)0.0812 (4)0.1280 (4)0.204 (4)
F6A0.2633 (11)0.1049 (16)0.0042 (11)0.216 (11)0.421 (17)
F7A0.3754 (16)0.0348 (8)0.0129 (11)0.149 (8)0.421 (17)
F8A0.3993 (17)0.1463 (9)0.0386 (12)0.149 (9)0.421 (17)
F6B0.4504 (8)0.0890 (11)0.0576 (10)0.202 (8)0.579 (17)
F7B0.3295 (13)0.1534 (6)0.0162 (9)0.167 (8)0.579 (17)
F8B0.3172 (11)0.0413 (7)0.0046 (9)0.176 (7)0.579 (17)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0436 (3)0.0330 (3)0.0329 (3)0.00020 (14)0.0169 (2)0.00079 (13)
N10.059 (3)0.031 (2)0.045 (2)0.0035 (19)0.021 (2)0.0014 (18)
C10.058 (3)0.035 (3)0.057 (3)0.005 (2)0.027 (3)0.003 (2)
N20.087 (4)0.031 (3)0.067 (3)0.008 (2)0.034 (3)0.002 (2)
C20.094 (5)0.041 (3)0.070 (4)0.001 (3)0.036 (4)0.013 (3)
C30.064 (3)0.059 (4)0.045 (3)0.005 (3)0.025 (3)0.006 (3)
N30.053 (2)0.043 (3)0.042 (2)0.0028 (19)0.018 (2)0.0011 (19)
C40.062 (3)0.039 (3)0.046 (3)0.003 (2)0.020 (3)0.005 (2)
N40.077 (3)0.046 (3)0.049 (3)0.007 (2)0.016 (2)0.010 (2)
C50.084 (4)0.068 (4)0.045 (3)0.008 (3)0.026 (3)0.009 (3)
C60.080 (4)0.050 (4)0.049 (3)0.001 (3)0.030 (3)0.006 (3)
N50.055 (2)0.041 (2)0.041 (2)0.0014 (19)0.022 (2)0.0005 (18)
C70.064 (3)0.043 (3)0.042 (3)0.005 (3)0.025 (3)0.001 (2)
N60.115 (5)0.052 (3)0.057 (3)0.008 (3)0.049 (3)0.006 (2)
C80.116 (6)0.067 (5)0.053 (4)0.006 (4)0.044 (4)0.000 (3)
C90.073 (4)0.054 (4)0.048 (3)0.003 (3)0.034 (3)0.001 (3)
N70.055 (2)0.039 (2)0.038 (2)0.0002 (19)0.0163 (19)0.0001 (18)
C100.067 (3)0.034 (3)0.050 (3)0.004 (2)0.025 (3)0.003 (2)
N80.115 (5)0.028 (3)0.056 (3)0.012 (3)0.034 (3)0.006 (2)
C110.112 (6)0.043 (4)0.057 (4)0.010 (3)0.032 (4)0.010 (3)
C120.069 (4)0.046 (3)0.039 (3)0.004 (3)0.018 (3)0.007 (2)
O10.052 (2)0.057 (3)0.052 (3)0.0021 (16)0.030 (2)0.0060 (17)
C130.051 (3)0.070 (4)0.064 (4)0.003 (3)0.020 (3)0.000 (3)
N90.066 (4)0.093 (5)0.070 (4)0.006 (3)0.049 (3)0.015 (3)
C140.096 (6)0.196 (13)0.131 (9)0.061 (8)0.069 (7)0.075 (9)
C150.106 (6)0.124 (8)0.104 (6)0.009 (6)0.070 (6)0.026 (6)
B10.125 (6)0.065 (5)0.059 (4)0.031 (5)0.029 (4)0.009 (3)
F10.190 (5)0.070 (3)0.084 (3)0.045 (3)0.033 (3)0.010 (2)
F2A0.144 (11)0.071 (6)0.065 (5)0.021 (6)0.026 (5)0.003 (4)
F3A0.124 (7)0.107 (11)0.141 (13)0.045 (7)0.012 (7)0.043 (10)
F4A0.207 (15)0.101 (7)0.114 (11)0.026 (8)0.077 (11)0.021 (7)
F2B0.096 (8)0.176 (18)0.130 (11)0.011 (10)0.027 (9)0.077 (12)
F3B0.126 (10)0.23 (2)0.143 (16)0.007 (11)0.067 (11)0.048 (13)
F4B0.31 (3)0.066 (7)0.087 (8)0.068 (12)0.062 (12)0.000 (6)
B2A0.173 (14)0.068 (12)0.114 (11)0.016 (11)0.060 (13)0.041 (13)
B2B0.193 (12)0.062 (10)0.097 (10)0.016 (10)0.051 (12)0.014 (9)
F50.363 (11)0.135 (6)0.136 (5)0.021 (6)0.118 (6)0.060 (4)
F6A0.185 (14)0.16 (2)0.252 (19)0.056 (12)0.026 (15)0.046 (16)
F7A0.23 (2)0.056 (8)0.185 (16)0.011 (10)0.106 (17)0.026 (9)
F8A0.27 (2)0.073 (10)0.141 (15)0.035 (14)0.119 (16)0.009 (10)
F6B0.162 (9)0.212 (19)0.198 (14)0.002 (10)0.025 (9)0.054 (13)
F7B0.261 (19)0.065 (6)0.140 (10)0.024 (9)0.035 (13)0.046 (6)
F8B0.218 (15)0.074 (8)0.171 (9)0.021 (9)0.002 (11)0.013 (7)
Geometric parameters (Å, º) top
Rh1—N72.041 (5)N7—C121.364 (7)
Rh1—N52.042 (4)C10—N81.339 (7)
Rh1—N32.049 (4)N8—C111.353 (9)
Rh1—N12.057 (4)N8—H8N0.8600
Rh1—O12.266 (5)C11—C121.366 (9)
Rh1—Rh1i2.6313 (18)C11—H110.9300
N1—C11.331 (7)C12—H120.9300
N1—C31.352 (7)O1—C131.216 (9)
C1—N21.337 (7)C13—N91.319 (9)
C1—C41.444 (8)C13—H130.9300
N2—C21.350 (8)N9—C141.439 (11)
N2—H2N0.8600N9—C151.458 (10)
C2—C31.358 (9)C14—H140.9600
C2—H20.9300C14—H14A0.9600
C3—H30.9300C14—H14B0.9600
N3—C41.328 (7)C15—H150.9600
N3—C61.363 (7)C15—H15A0.9600
C4—N41.331 (7)C15—H15B0.9600
N4—C51.365 (8)B1—F2B1.300 (11)
N4—H4N0.8600B1—F3A1.306 (10)
C5—C61.348 (9)B1—F11.338 (8)
C5—H50.9300B1—F4B1.349 (10)
C6—H60.9300B1—F2A1.389 (10)
N5—C71.336 (7)B1—F4A1.408 (11)
N5—C91.368 (7)B1—F3B1.412 (12)
C7—N61.332 (7)B2A—F51.330 (13)
C7—C101.442 (8)B2A—F6A1.333 (14)
N6—C81.357 (8)B2A—F8A1.341 (14)
N6—H6N0.8600B2A—F7A1.344 (14)
C8—C91.348 (9)B2B—F51.324 (13)
C8—H80.9300B2B—F7B1.331 (13)
C9—H90.9300B2B—F8B1.333 (13)
N7—C101.324 (7)B2B—F6B1.350 (13)
N7—Rh1—N579.88 (18)N5—C9—H9125.7
N7—Rh1—N399.97 (18)C10—N7—C12106.4 (5)
N5—Rh1—N3173.40 (17)C10—N7—Rh1113.3 (4)
N7—Rh1—N1175.25 (17)C12—N7—Rh1139.9 (4)
N5—Rh1—N199.96 (18)N7—C10—N8111.1 (5)
N3—Rh1—N179.63 (18)N7—C10—C7116.3 (5)
N7—Rh1—O184.66 (16)N8—C10—C7132.5 (6)
N5—Rh1—O184.44 (17)C10—N8—C11106.9 (5)
N3—Rh1—O188.97 (17)C10—N8—H8N126.6
N1—Rh1—O190.60 (16)C11—N8—H8N126.6
N7—Rh1—Rh1i92.08 (13)N8—C11—C12107.5 (5)
N5—Rh1—Rh1i93.04 (13)N8—C11—H11126.3
N3—Rh1—Rh1i93.55 (13)C12—C11—H11126.3
N1—Rh1—Rh1i92.67 (13)N7—C12—C11108.1 (5)
O1—Rh1—Rh1i176.18 (10)N7—C12—H12125.9
C1—N1—C3105.8 (5)C11—C12—H12125.9
C1—N1—Rh1113.2 (4)C13—O1—Rh1115.8 (4)
C3—N1—Rh1140.8 (4)O1—C13—N9124.7 (7)
N1—C1—N2111.1 (5)O1—C13—H13117.7
N1—C1—C4116.7 (5)N9—C13—H13117.7
N2—C1—C4132.1 (6)C13—N9—C14119.4 (7)
C1—N2—C2106.7 (5)C13—N9—C15121.4 (7)
C1—N2—H2N126.6C14—N9—C15119.2 (7)
C2—N2—H2N126.6N9—C14—H14109.5
N2—C2—C3107.3 (5)N9—C14—H14A109.5
N2—C2—H2126.3H14—C14—H14A109.5
C3—C2—H2126.3N9—C14—H14B109.5
N1—C3—C2109.0 (5)H14—C14—H14B109.5
N1—C3—H3125.5H14A—C14—H14B109.5
C2—C3—H3125.5N9—C15—H15109.5
C4—N3—C6105.8 (5)N9—C15—H15A109.5
C4—N3—Rh1113.7 (4)H15—C15—H15A109.5
C6—N3—Rh1139.6 (4)N9—C15—H15B109.5
N3—C4—N4111.2 (5)H15—C15—H15B109.5
N3—C4—C1116.2 (5)H15A—C15—H15B109.5
N4—C4—C1132.6 (6)F2B—B1—F1118.2 (10)
C4—N4—C5106.8 (5)F3A—B1—F1119.1 (9)
C4—N4—H4N126.6F2B—B1—F4B114.8 (11)
C5—N4—H4N126.6F1—B1—F4B107.1 (7)
C6—C5—N4107.1 (5)F3A—B1—F2A109.5 (9)
C6—C5—H5126.5F1—B1—F2A109.7 (7)
N4—C5—H5126.5F3A—B1—F4A107.2 (8)
C5—C6—N3109.0 (6)F1—B1—F4A106.6 (8)
C5—C6—H6125.5F2A—B1—F4A103.5 (9)
N3—C6—H6125.5F2B—B1—F3B106.0 (10)
C7—N5—C9106.1 (5)F1—B1—F3B104.4 (9)
C7—N5—Rh1112.7 (3)F4B—B1—F3B105.0 (9)
C9—N5—Rh1139.2 (4)F5—B2A—F6A111.6 (13)
N6—C7—N5110.4 (5)F5—B2A—F8A109.3 (12)
N6—C7—C10133.3 (6)F6A—B2A—F8A109.5 (13)
N5—C7—C10116.3 (5)F5—B2A—F7A108.9 (12)
C7—N6—C8107.5 (5)F6A—B2A—F7A109.0 (13)
C7—N6—H6N126.2F8A—B2A—F7A108.4 (12)
C8—N6—H6N126.2F5—B2B—F7B111.9 (12)
C9—C8—N6107.4 (6)F5—B2B—F8B108.9 (12)
C9—C8—H8126.3F7B—B2B—F8B108.8 (12)
N6—C8—H8126.3F5—B2B—F6B107.7 (11)
C8—C9—N5108.6 (6)F7B—B2B—F6B109.3 (12)
C8—C9—H9125.7F8B—B2B—F6B110.2 (12)
N1—Rh1—Rh1i—N3i43.72 (18)O1—Rh1—N5—C774.8 (4)
N5—Rh1—Rh1i—N7i43.72 (17)Rh1i—Rh1—N5—C7102.3 (4)
N7—Rh1—N1—C181 (2)N7—Rh1—N5—C9171.5 (6)
N5—Rh1—N1—C1169.0 (4)N3—Rh1—N5—C982.2 (16)
N3—Rh1—N1—C14.3 (4)N1—Rh1—N5—C93.7 (6)
O1—Rh1—N1—C184.5 (4)O1—Rh1—N5—C985.9 (6)
Rh1i—Rh1—N1—C197.4 (4)Rh1i—Rh1—N5—C997.0 (6)
N7—Rh1—N1—C393 (2)C9—N5—C7—N61.2 (7)
N5—Rh1—N1—C35.4 (7)Rh1—N5—C7—N6168.2 (4)
N3—Rh1—N1—C3178.7 (7)C9—N5—C7—C10177.3 (5)
O1—Rh1—N1—C389.8 (6)Rh1—N5—C7—C1010.3 (7)
Rh1i—Rh1—N1—C388.2 (6)N5—C7—N6—C80.0 (8)
C3—N1—C1—N20.4 (7)C10—C7—N6—C8178.1 (7)
Rh1—N1—C1—N2176.7 (4)C7—N6—C8—C91.2 (9)
C3—N1—C1—C4178.4 (5)N6—C8—C9—N51.9 (8)
Rh1—N1—C1—C42.1 (7)C7—N5—C9—C81.9 (7)
N1—C1—N2—C20.3 (8)Rh1—N5—C9—C8163.4 (5)
C4—C1—N2—C2178.8 (7)N5—Rh1—N7—C109.7 (4)
C1—N2—C2—C30.9 (8)N3—Rh1—N7—C10163.6 (4)
C1—N1—C3—C21.0 (7)N1—Rh1—N7—C1079 (2)
Rh1—N1—C3—C2175.6 (5)O1—Rh1—N7—C1075.6 (4)
N2—C2—C3—N11.2 (8)Rh1i—Rh1—N7—C10102.4 (4)
N7—Rh1—N3—C4169.1 (4)N5—Rh1—N7—C12179.1 (6)
N5—Rh1—N3—C481.0 (15)N3—Rh1—N7—C127.5 (6)
N1—Rh1—N3—C46.1 (4)N1—Rh1—N7—C1292 (2)
O1—Rh1—N3—C484.7 (4)O1—Rh1—N7—C1295.6 (6)
Rh1i—Rh1—N3—C498.2 (4)Rh1i—Rh1—N7—C1286.4 (6)
N7—Rh1—N3—C61.4 (7)C12—N7—C10—N80.4 (7)
N5—Rh1—N3—C686.7 (16)Rh1—N7—C10—N8173.7 (4)
N1—Rh1—N3—C6173.8 (7)C12—N7—C10—C7178.7 (5)
O1—Rh1—N3—C683.0 (6)Rh1—N7—C10—C77.2 (7)
Rh1i—Rh1—N3—C694.2 (6)N6—C7—C10—N7175.9 (7)
C6—N3—C4—N40.2 (7)N5—C7—C10—N72.1 (8)
Rh1—N3—C4—N4171.9 (4)N6—C7—C10—N85.1 (13)
C6—N3—C4—C1178.6 (5)N5—C7—C10—N8176.8 (7)
Rh1—N3—C4—C16.9 (7)N7—C10—N8—C110.5 (8)
N1—C1—C4—N33.2 (8)C7—C10—N8—C11178.5 (7)
N2—C1—C4—N3178.3 (6)C10—N8—C11—C120.3 (9)
N1—C1—C4—N4175.2 (6)C10—N7—C12—C110.2 (7)
N2—C1—C4—N43.3 (12)Rh1—N7—C12—C11171.3 (5)
N3—C4—N4—C50.0 (7)N8—C11—C12—N70.1 (8)
C1—C4—N4—C5178.5 (7)N7—Rh1—O1—C13136.6 (5)
C4—N4—C5—C60.2 (7)N5—Rh1—O1—C1356.3 (5)
N4—C5—C6—N30.3 (8)N3—Rh1—O1—C13123.3 (5)
C4—N3—C6—C50.3 (7)N1—Rh1—O1—C1343.7 (5)
Rh1—N3—C6—C5168.5 (5)Rh1i—Rh1—O1—C13105.3 (17)
N7—Rh1—N5—C710.7 (4)Rh1—O1—C13—N9163.8 (6)
N3—Rh1—N5—C778.6 (15)O1—C13—N9—C143.6 (13)
N1—Rh1—N5—C7164.4 (4)O1—C13—N9—C15177.8 (8)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···F50.861.932.786 (8)170
N4—H4N···F8B0.861.972.818 (15)171
N4—H4N···F7A0.861.982.738 (17)146
N6—H6N···F4B0.861.942.773 (13)163
N6—H6N···F4A0.862.092.927 (16)166
N6—H6N···F3A0.862.543.19 (2)134
N8—H8N···F2A0.861.972.817 (15)167
N8—H8N···F2B0.862.082.884 (19)155
N8—H8N···F3B0.862.433.169 (19)144
N8—H8N···F3A0.862.563.227 (15)136
(V) top
Crystal data top
C36H38N18Rh2·2(SiF6)·8(H2O)Dx = 1.726 Mg m3
Mr = 1356.97Mo Kα radiation, λ = 0.71069 Å
Tetragonal, I4122Cell parameters from 14243 reflections
a = 17.6300 (5) Åθ = 3.0–27.5°
c = 16.8037 (6) ŵ = 0.79 mm1
V = 5222.9 (3) Å3T = 296 K
Z = 4Prismatic, red
F(000) = 27440.41 × 0.40 × 0.40 mm
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
3004 independent reflections
Radiation source: rotating-anode X-ray tube2952 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.024
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.3°
ω scansh = 2221
Absorption correction: numerical
NUMABS (Higashi, 1999)
k = 2222
Tmin = 0.727, Tmax = 0.814l = 1421
20508 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.073 w = 1/[σ2(Fo2) + (0.0493P)2 + 1.975P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max = 0.001
3004 reflectionsΔρmax = 0.80 e Å3
220 parametersΔρmin = 0.36 e Å3
15 restraintsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (3)
Crystal data top
C36H38N18Rh2·2(SiF6)·8(H2O)Z = 4
Mr = 1356.97Mo Kα radiation
Tetragonal, I4122µ = 0.79 mm1
a = 17.6300 (5) ÅT = 296 K
c = 16.8037 (6) Å0.41 × 0.40 × 0.40 mm
V = 5222.9 (3) Å3
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
3004 independent reflections
Absorption correction: numerical
NUMABS (Higashi, 1999)
2952 reflections with I > 2σ(I)
Tmin = 0.727, Tmax = 0.814Rint = 0.024
20508 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.027H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.073Δρmax = 0.80 e Å3
S = 1.12Δρmin = 0.36 e Å3
3004 reflectionsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
220 parametersAbsolute structure parameter: 0.02 (3)
15 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 not 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
xyzUiso*/UeqOcc. (<1)
Rh10.445750 (10)0.445750 (10)0.00000.02735 (9)
N10.36851 (12)0.51661 (12)0.05284 (12)0.0312 (4)
C10.36143 (16)0.50496 (15)0.13091 (16)0.0367 (5)
N20.30158 (14)0.54327 (15)0.15982 (15)0.0441 (5)
H2N0.28660.54400.20850.053*
C20.26894 (16)0.58083 (16)0.09758 (19)0.0423 (6)
H20.22630.61180.09990.051*
C30.31059 (14)0.56455 (15)0.03147 (18)0.0365 (5)
H30.30140.58280.01950.044*
N30.46441 (13)0.42079 (13)0.11796 (13)0.0353 (4)
C40.41519 (17)0.45467 (15)0.16714 (15)0.0387 (5)
N40.42891 (19)0.43573 (15)0.24257 (14)0.0550 (6)
H4N0.40470.45160.28380.066*
C50.4885 (2)0.3865 (2)0.2420 (2)0.0606 (9)
H50.51040.36360.28630.073*
C60.5098 (2)0.37689 (17)0.16603 (18)0.0465 (6)
H60.54900.34560.14870.056*
N50.35452 (13)0.35452 (13)0.00000.0423 (6)
C70.3687 (2)0.2847 (3)0.0156 (5)0.124 (3)
H70.41870.27140.02660.148*
C80.3152 (3)0.2287 (3)0.0172 (6)0.157 (4)
H80.32980.17960.03070.189*
C90.2425 (2)0.2425 (2)0.00000.0865 (19)
C100.1817 (3)0.1817 (3)0.00000.163 (6)
H10A0.13400.20380.01500.245*0.50
H10B0.17760.16020.05230.245*0.50
H10C0.19510.14270.03730.245*0.50
Si10.22790 (15)0.54844 (14)0.3697 (2)0.0739 (10)0.50
F10.1635 (7)0.4809 (4)0.3825 (6)0.146 (4)0.50
F20.2708 (7)0.5186 (7)0.4520 (4)0.128 (4)0.50
F30.2914 (7)0.6168 (6)0.3578 (7)0.149 (4)0.50
F40.2837 (6)0.4894 (4)0.3167 (4)0.096 (2)0.50
F50.1905 (6)0.5772 (7)0.2878 (4)0.131 (3)0.50
F60.1762 (6)0.6065 (5)0.4258 (5)0.114 (3)0.50
O10.34398 (18)0.75000.12500.0542 (7)
O20.23366 (16)0.73366 (16)0.25000.0739 (10)
O40.4094 (13)0.4941 (15)0.5655 (11)0.270 (11)0.50
O30.4212 (10)0.4807 (14)0.3987 (10)0.242 (10)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.03114 (10)0.03114 (10)0.01978 (12)0.00846 (8)0.00059 (6)0.00059 (6)
N10.0344 (10)0.0350 (10)0.0241 (9)0.0057 (8)0.0019 (8)0.0024 (7)
C10.0447 (13)0.0372 (12)0.0282 (12)0.0073 (11)0.0093 (10)0.0024 (10)
N20.0462 (12)0.0473 (13)0.0388 (13)0.0053 (10)0.0173 (10)0.0091 (10)
C20.0355 (12)0.0398 (13)0.0517 (17)0.0075 (10)0.0066 (12)0.0097 (12)
C30.0339 (11)0.0322 (12)0.0434 (13)0.0047 (9)0.0044 (10)0.0007 (10)
N30.0436 (11)0.0369 (10)0.0255 (10)0.0085 (9)0.0007 (8)0.0007 (8)
C40.0529 (14)0.0397 (13)0.0234 (11)0.0061 (11)0.0068 (10)0.0002 (10)
N40.0895 (19)0.0537 (14)0.0219 (10)0.0183 (11)0.0079 (12)0.0059 (10)
C50.091 (2)0.0585 (17)0.0322 (16)0.0159 (17)0.0100 (17)0.0105 (15)
C60.0608 (18)0.0420 (15)0.0368 (14)0.0142 (12)0.0055 (13)0.0068 (12)
N50.0424 (9)0.0424 (9)0.0421 (16)0.0122 (12)0.0013 (11)0.0013 (11)
C70.0434 (18)0.068 (3)0.260 (9)0.0111 (17)0.022 (3)0.080 (4)
C80.063 (2)0.063 (2)0.347 (13)0.0024 (19)0.011 (5)0.086 (5)
C90.0553 (16)0.0553 (16)0.149 (6)0.006 (2)0.008 (3)0.008 (3)
C100.087 (4)0.087 (4)0.316 (17)0.044 (4)0.042 (8)0.042 (8)
Si10.115 (3)0.0649 (11)0.0414 (12)0.0008 (13)0.028 (2)0.0082 (11)
F10.207 (11)0.115 (6)0.116 (6)0.060 (7)0.097 (8)0.005 (5)
F20.167 (10)0.170 (10)0.047 (4)0.078 (8)0.031 (5)0.001 (5)
F30.178 (10)0.093 (5)0.175 (12)0.025 (6)0.051 (8)0.005 (7)
F40.146 (7)0.088 (4)0.053 (4)0.004 (5)0.043 (4)0.001 (3)
F50.158 (8)0.171 (8)0.064 (4)0.007 (6)0.019 (4)0.034 (5)
F60.158 (9)0.103 (5)0.079 (5)0.051 (6)0.021 (5)0.008 (4)
O10.0447 (16)0.0604 (18)0.0574 (18)0.0000.0000.0204 (14)
O20.0829 (16)0.0829 (16)0.0561 (19)0.0102 (19)0.0072 (16)0.0072 (16)
O40.28 (2)0.39 (3)0.144 (14)0.09 (2)0.007 (15)0.026 (18)
O30.173 (13)0.39 (3)0.158 (13)0.105 (17)0.023 (10)0.118 (15)
Geometric parameters (Å, º) top
Rh1—N1i2.0502 (19)C5—C61.342 (5)
Rh1—N12.0502 (18)C5—H50.9300
Rh1—N3i2.057 (2)C6—H60.9300
Rh1—N32.057 (2)N5—C7i1.283 (4)
Rh1—N52.275 (3)N5—C71.283 (4)
Rh1—Rh1ii2.7052 (5)C7—C81.367 (7)
N1—C11.334 (3)C7—H70.9300
N1—C31.373 (3)C8—C91.337 (6)
C1—N21.344 (3)C8—H80.9300
C1—C41.434 (4)C9—C8i1.337 (6)
N2—C21.365 (4)C9—C101.514 (8)
N2—H2N0.8600C10—H10A0.9600
C2—C31.362 (4)C10—H10B0.9600
C2—H20.9300C10—H10C0.9600
C3—H30.9300Si1—F51.607 (8)
N3—C41.339 (3)Si1—F31.658 (10)
N3—C61.376 (3)Si1—F11.659 (8)
C4—N41.333 (3)Si1—F21.662 (8)
N4—C51.363 (5)Si1—F61.664 (7)
N4—H4N0.8600Si1—F41.687 (7)
N1i—Rh1—N1175.55 (12)C6—C5—N4107.6 (3)
N1i—Rh1—N3i79.59 (8)C6—C5—H5126.2
N1—Rh1—N3i100.24 (8)N4—C5—H5126.2
N1i—Rh1—N3100.24 (8)C5—C6—N3108.9 (3)
N1—Rh1—N379.59 (8)C5—C6—H6125.5
N3i—Rh1—N3175.62 (13)N3—C6—H6125.5
N1i—Rh1—N587.78 (6)C7i—N5—C7114.6 (5)
N1—Rh1—N587.78 (6)C7i—N5—Rh1122.7 (2)
N3i—Rh1—N587.81 (7)C7—N5—Rh1122.7 (2)
N3—Rh1—N587.81 (7)N5—C7—C8124.2 (4)
N1i—Rh1—Rh1ii92.22 (6)N5—C7—H7117.9
N1—Rh1—Rh1ii92.23 (6)C8—C7—H7117.9
N3i—Rh1—Rh1ii92.19 (7)C9—C8—C7121.8 (4)
N3—Rh1—Rh1ii92.19 (7)C9—C8—H8119.1
N5—Rh1—Rh1ii180.0C7—C8—H8119.1
C1—N1—C3106.4 (2)C8—C9—C8i113.3 (5)
C1—N1—Rh1113.22 (16)C8—C9—C10123.3 (3)
C3—N1—Rh1139.08 (18)C8i—C9—C10123.3 (3)
N1—C1—N2110.6 (3)C9—C10—H10A109.5
N1—C1—C4116.8 (2)C9—C10—H10B109.5
N2—C1—C4132.6 (3)H10A—C10—H10B109.5
C1—N2—C2107.3 (2)C9—C10—H10C109.5
C1—N2—H2N126.3H10A—C10—H10C109.5
C2—N2—H2N126.3H10B—C10—H10C109.5
C3—C2—N2107.2 (2)F5—Si1—F386.8 (6)
C3—C2—H2126.4F5—Si1—F193.3 (6)
N2—C2—H2126.4F3—Si1—F1179.1 (6)
C2—C3—N1108.5 (2)F5—Si1—F2177.1 (5)
C2—C3—H3125.8F3—Si1—F291.3 (8)
N1—C3—H3125.8F1—Si1—F288.6 (7)
C4—N3—C6105.4 (2)F5—Si1—F693.8 (5)
C4—N3—Rh1113.30 (17)F3—Si1—F689.5 (6)
C6—N3—Rh1141.2 (2)F1—Si1—F689.6 (5)
N4—C4—N3111.0 (3)F2—Si1—F688.4 (4)
N4—C4—C1132.7 (3)F5—Si1—F489.0 (5)
N3—C4—C1116.3 (2)F3—Si1—F489.5 (5)
C4—N4—C5107.0 (3)F1—Si1—F491.4 (4)
C4—N4—H4N126.5F2—Si1—F488.8 (4)
C5—N4—H4N126.5F6—Si1—F4177.0 (6)
N1—Rh1ii—Rh1ii—N3Rh1ii—Rh1—N3—C686.0 (3)
N1i—Rh1—N1—C179.98 (19)C6—N3—C4—N41.6 (3)
N3i—Rh1—N1—C1167.35 (19)Rh1—N3—C4—N4179.0 (2)
N3—Rh1—N1—C18.20 (19)C6—N3—C4—C1179.3 (3)
N5—Rh1—N1—C179.98 (19)Rh1—N3—C4—C13.3 (3)
Rh1ii—Rh1—N1—C1100.02 (19)N1—C1—C4—N4173.2 (3)
N1i—Rh1—N1—C384.6 (3)N2—C1—C4—N48.7 (6)
N3i—Rh1—N1—C32.7 (3)N1—C1—C4—N33.9 (4)
N3—Rh1—N1—C3172.8 (3)N2—C1—C4—N3174.2 (3)
N5—Rh1—N1—C384.6 (3)N3—C4—N4—C51.2 (4)
Rh1ii—Rh1—N1—C395.4 (3)C1—C4—N4—C5178.4 (3)
C3—N1—C1—N20.1 (3)C4—N4—C5—C60.3 (4)
Rh1—N1—C1—N2169.46 (19)N4—C5—C6—N30.7 (4)
C3—N1—C1—C4178.6 (2)C4—N3—C6—C51.4 (4)
Rh1—N1—C1—C49.0 (3)Rh1—N3—C6—C5177.6 (3)
N1—C1—N2—C20.1 (3)N1i—Rh1—N5—C7i140.2 (5)
C4—C1—N2—C2178.0 (3)N1—Rh1—N5—C7i39.8 (5)
C1—N2—C2—C30.3 (3)N3i—Rh1—N5—C7i60.6 (5)
N2—C2—C3—N10.4 (3)N3—Rh1—N5—C7i119.4 (5)
C1—N1—C3—C20.3 (3)Rh1ii—Rh1—N5—C7i165.9 (5)
Rh1—N1—C3—C2165.0 (2)N1i—Rh1—N5—C739.8 (5)
N1i—Rh1—N3—C4169.34 (19)N1—Rh1—N5—C7140.2 (5)
N1—Rh1—N3—C46.14 (19)N3i—Rh1—N5—C7119.4 (5)
N3i—Rh1—N3—C482.00 (19)N3—Rh1—N5—C760.6 (5)
N5—Rh1—N3—C482.00 (19)Rh1ii—Rh1—N5—C714.1 (5)
Rh1ii—Rh1—N3—C498.00 (19)C7i—N5—C7—C80.9 (7)
N1i—Rh1—N3—C66.6 (4)Rh1—N5—C7—C8179.1 (7)
N1—Rh1—N3—C6177.9 (4)N5—C7—C8—C92.0 (14)
N3i—Rh1—N3—C694.0 (3)C7—C8—C9—C8i0.9 (6)
N5—Rh1—N3—C694.0 (3)C7—C8—C9—C10179.1 (6)
Symmetry codes: (i) y, x, z; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···F2iii0.861.872.684 (7)158
N2—H2N···F40.862.062.819 (8)147
N2—H2N···F50.862.232.970 (10)144
N2—H2N···F6iii0.862.333.004 (9)136
N4—H4N···F1iii0.861.922.774 (7)171
N4—H4N···F40.862.302.999 (9)138
N4—H4N···O30.862.022.744 (14)141
Symmetry code: (iii) x+1/2, y, z+3/4.
(VI) top
Crystal data top
C60H60N38Rh4·SiF6·6(ClO4)·12.7(H2O)Dx = 1.777 Mg m3
Mr = 2692.69Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, PbcaCell parameters from 25234 reflections
a = 20.170 (2) Åθ = 3.3–27.5°
b = 21.875 (3) ŵ = 0.94 mm1
c = 22.541 (3) ÅT = 296 K
V = 9946 (2) Å3Prismatic, red
Z = 40.50 × 0.42 × 0.31 mm
F(000) = 5420
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
11352 independent reflections
Radiation source: rotating-anode X-ray tube10339 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.3°
ω scansh = 2624
Absorption correction: numerical
NUMABS (Higashi, 1999)
k = 2827
Tmin = 0.832, Tmax = 0.894l = 2229
71587 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.059Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.180H atoms treated by a mixture of independent and constrained refinement
S = 1.17 w = 1/[σ2(Fo2) + (0.0782P)2 + 29.1806P]
where P = (Fo2 + 2Fc2)/3
11379 reflections(Δ/σ)max = 0.002
712 parametersΔρmax = 1.65 e Å3
12 restraintsΔρmin = 1.44 e Å3
Crystal data top
C60H60N38Rh4·SiF6·6(ClO4)·12.7(H2O)V = 9946 (2) Å3
Mr = 2692.69Z = 4
Orthorhombic, PbcaMo Kα radiation
a = 20.170 (2) ŵ = 0.94 mm1
b = 21.875 (3) ÅT = 296 K
c = 22.541 (3) Å0.50 × 0.42 × 0.31 mm
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
11352 independent reflections
Absorption correction: numerical
NUMABS (Higashi, 1999)
10339 reflections with I > 2σ(I)
Tmin = 0.832, Tmax = 0.894Rint = 0.035
71587 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05912 restraints
wR(F2) = 0.180H atoms treated by a mixture of independent and constrained refinement
S = 1.17 w = 1/[σ2(Fo2) + (0.0782P)2 + 29.1806P]
where P = (Fo2 + 2Fc2)/3
11379 reflectionsΔρmax = 1.65 e Å3
712 parametersΔρmin = 1.44 e Å3
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 not 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
xyzUiso*/UeqOcc. (<1)
Rh10.285008 (17)0.702100 (16)0.559554 (17)0.03460 (12)
Rh20.376560 (16)0.616341 (15)0.534188 (16)0.03148 (11)
N10.3360 (2)0.76822 (18)0.5135 (2)0.0413 (9)
C10.3731 (3)0.8043 (2)0.5486 (3)0.0506 (14)
N20.3990 (3)0.8501 (2)0.5177 (3)0.0626 (14)
H2N0.42390.87870.53150.075*
C20.3789 (3)0.8436 (3)0.4604 (4)0.0656 (18)
H20.39020.86880.42870.079*
C30.3394 (3)0.7937 (3)0.4580 (3)0.0545 (14)
H30.31800.77900.42430.065*
N30.3427 (2)0.7378 (2)0.6263 (2)0.0458 (10)
C40.3773 (3)0.7869 (3)0.6097 (3)0.0501 (13)
N40.4128 (3)0.8083 (3)0.6558 (3)0.0730 (17)
H4N0.43920.83920.65550.088*
C50.3990 (4)0.7722 (4)0.7025 (4)0.079 (2)
H50.41640.77650.74050.095*
C60.3562 (4)0.7291 (3)0.6854 (3)0.0631 (17)
H60.33870.69850.70930.076*
N50.2228 (2)0.66996 (19)0.4944 (2)0.0429 (9)
C70.1756 (3)0.6327 (2)0.5148 (3)0.0510 (14)
N60.1355 (3)0.6166 (2)0.4703 (3)0.0705 (18)
H6N0.10170.59270.47290.085*
C80.1569 (4)0.6441 (3)0.4209 (4)0.0706 (19)
H80.13770.64090.38350.085*
C90.2110 (3)0.6775 (3)0.4346 (3)0.0528 (14)
H90.23580.70120.40860.063*
N70.2288 (2)0.6413 (2)0.6074 (2)0.0501 (11)
C100.1784 (3)0.6188 (3)0.5767 (4)0.0589 (16)
N80.1395 (3)0.5844 (3)0.6119 (4)0.080 (2)
H8N0.10470.56450.60130.095*
C110.1657 (4)0.5870 (4)0.6673 (4)0.085 (3)
H110.14860.56810.70090.102*
C120.2208 (4)0.6218 (3)0.6650 (3)0.0684 (19)
H120.24850.63100.69670.082*
N90.4529 (2)0.67712 (17)0.5442 (2)0.0386 (9)
C130.4819 (3)0.6748 (2)0.5972 (3)0.0441 (11)
N100.5328 (2)0.7140 (2)0.5997 (3)0.0558 (12)
H10N0.55820.72050.62970.067*
C140.5368 (3)0.7418 (3)0.5457 (3)0.0593 (15)
H140.56770.77120.53460.071*
C150.4883 (3)0.7190 (2)0.5112 (3)0.0483 (12)
H150.48000.72960.47200.058*
N110.3992 (2)0.60354 (19)0.6218 (2)0.0406 (9)
C160.4538 (3)0.6336 (2)0.6395 (2)0.0442 (11)
N120.4687 (3)0.6182 (2)0.6952 (2)0.0594 (13)
H12N0.50120.63250.71560.071*
C170.4242 (4)0.5764 (3)0.7142 (3)0.0635 (16)
H170.42330.55760.75120.076*
C180.3805 (3)0.5670 (3)0.6687 (3)0.0530 (13)
H180.34450.54050.66930.064*
N130.3605 (2)0.62420 (18)0.44503 (19)0.0384 (9)
C190.3217 (3)0.5808 (2)0.4229 (2)0.0438 (11)
N140.3198 (3)0.5833 (3)0.3638 (2)0.0680 (15)
H14N0.29750.55980.34060.082*
C200.3604 (4)0.6306 (3)0.3470 (3)0.0718 (19)
H200.36940.64290.30830.086*
C210.3847 (3)0.6560 (3)0.3971 (3)0.0540 (13)
H210.41310.68940.39890.065*
N150.30583 (19)0.54976 (18)0.52193 (19)0.0380 (8)
C220.2900 (3)0.5411 (2)0.4654 (2)0.0432 (11)
N160.2459 (3)0.4958 (2)0.4603 (3)0.0556 (12)
H16N0.22840.48270.42800.067*
C230.2340 (3)0.4744 (3)0.5157 (3)0.0571 (15)
H230.20580.44230.52550.069*
C240.2701 (3)0.5075 (2)0.5537 (3)0.0481 (12)
H240.27090.50270.59470.058*
N170.2080 (2)0.77348 (19)0.5770 (2)0.0437 (10)
C250.1788 (4)0.7800 (3)0.6296 (3)0.0644 (17)
H250.19090.75450.66080.077*
C260.1309 (4)0.8240 (4)0.6385 (4)0.085 (3)
H260.11190.82750.67590.102*
N180.1107 (3)0.8616 (3)0.5956 (3)0.0786 (18)
C270.1400 (4)0.8545 (3)0.5440 (3)0.0680 (18)
H270.12770.87990.51290.082*
C280.1882 (3)0.8112 (3)0.5342 (3)0.0530 (13)
H280.20740.80820.49680.064*
N190.45273 (18)0.54441 (17)0.51296 (19)0.0361 (8)
C290.4560 (3)0.4916 (2)0.5429 (2)0.0421 (11)
H290.42580.48420.57320.051*
C300.4973 (2)0.5519 (2)0.4700 (2)0.0406 (11)
H300.49680.58790.44800.049*
Cl10.2778 (2)0.58238 (11)0.19874 (16)0.1522 (17)
O10.2233 (6)0.5459 (5)0.1986 (7)0.218 (6)
O20.3269 (9)0.5550 (5)0.2311 (6)0.286 (10)
O30.2965 (8)0.5927 (6)0.1370 (5)0.235 (7)
O40.2651 (5)0.6388 (4)0.2261 (5)0.164 (4)
Cl20.50273 (10)0.69105 (11)0.83968 (9)0.0785 (5)
O50.4665 (8)0.6378 (7)0.8369 (5)0.256 (9)
O60.5326 (4)0.6946 (4)0.8946 (3)0.122 (3)
O70.4637 (8)0.7368 (7)0.8328 (5)0.267 (9)
O80.5462 (3)0.6853 (4)0.7924 (3)0.113 (2)
Cl30.64557 (13)0.59097 (13)0.63762 (11)0.0989 (8)
O90.6837 (6)0.6371 (5)0.6036 (5)0.188 (5)
O100.6148 (3)0.6242 (4)0.6822 (3)0.117 (3)
O110.6952 (4)0.5514 (3)0.6597 (4)0.124 (3)
O120.6029 (4)0.5617 (5)0.6002 (5)0.161 (4)
Si10.00000.50000.50000.0809 (10)
F10.0061 (3)0.5712 (3)0.4753 (6)0.196 (5)
F20.0731 (3)0.4893 (3)0.4715 (5)0.172 (4)
F30.0333 (6)0.5196 (6)0.5631 (5)0.243 (6)
O1W0.3069 (5)0.8489 (5)0.3071 (4)0.149 (3)
O2W0.2339 (5)0.7416 (4)0.3008 (4)0.145 (3)
O3W0.5974 (4)0.7635 (3)0.7008 (3)0.103 (2)
O4W0.1611 (6)0.4761 (5)0.3607 (5)0.191 (5)
O5W0.5199 (19)0.8690 (15)0.701 (2)0.15 (2)0.26 (3)
O6W0.6244 (17)0.9272 (13)0.7204 (11)0.233 (12)0.50
O7W0.4936 (11)0.9107 (10)0.6510 (13)0.303 (17)0.74 (3)
O8W0.4435 (18)0.5109 (17)0.2650 (18)0.29 (3)0.50 (4)
O9W0.5150 (19)0.5739 (16)0.2977 (16)0.20 (2)0.35 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0332 (2)0.03079 (19)0.0399 (2)0.00056 (13)0.00202 (14)0.00012 (13)
Rh20.03014 (19)0.02803 (18)0.0363 (2)0.00111 (12)0.00235 (13)0.00109 (13)
N10.038 (2)0.034 (2)0.052 (3)0.0003 (16)0.0027 (18)0.0032 (17)
C10.038 (3)0.036 (3)0.078 (4)0.001 (2)0.001 (3)0.007 (3)
N20.050 (3)0.039 (2)0.099 (5)0.008 (2)0.010 (3)0.004 (3)
C20.069 (4)0.045 (3)0.083 (5)0.002 (3)0.018 (4)0.015 (3)
C30.062 (4)0.045 (3)0.056 (3)0.003 (3)0.012 (3)0.005 (2)
N30.047 (2)0.042 (2)0.049 (3)0.0094 (18)0.0012 (19)0.0065 (19)
C40.045 (3)0.042 (3)0.063 (4)0.003 (2)0.010 (2)0.013 (2)
N40.067 (4)0.060 (3)0.092 (5)0.004 (3)0.023 (3)0.030 (3)
C50.092 (5)0.084 (5)0.061 (4)0.023 (4)0.024 (4)0.024 (4)
C60.081 (4)0.065 (4)0.043 (3)0.026 (3)0.004 (3)0.011 (3)
N50.036 (2)0.038 (2)0.055 (3)0.0017 (16)0.0005 (18)0.0040 (18)
C70.032 (2)0.040 (3)0.081 (4)0.006 (2)0.004 (3)0.009 (3)
N60.041 (3)0.054 (3)0.116 (6)0.010 (2)0.019 (3)0.010 (3)
C80.063 (4)0.071 (4)0.078 (5)0.006 (3)0.025 (4)0.020 (4)
C90.050 (3)0.054 (3)0.054 (3)0.004 (2)0.011 (2)0.007 (3)
N70.048 (2)0.039 (2)0.063 (3)0.0046 (19)0.019 (2)0.007 (2)
C100.040 (3)0.042 (3)0.094 (5)0.003 (2)0.021 (3)0.006 (3)
N80.061 (3)0.056 (3)0.122 (6)0.010 (3)0.038 (4)0.015 (4)
C110.086 (5)0.067 (4)0.104 (7)0.008 (4)0.049 (5)0.031 (4)
C120.079 (5)0.057 (4)0.069 (4)0.015 (3)0.030 (4)0.017 (3)
N90.037 (2)0.0292 (18)0.050 (2)0.0010 (15)0.0033 (17)0.0020 (16)
C130.039 (2)0.041 (3)0.052 (3)0.001 (2)0.003 (2)0.005 (2)
N100.039 (2)0.060 (3)0.069 (3)0.012 (2)0.005 (2)0.013 (2)
C140.048 (3)0.049 (3)0.082 (4)0.013 (3)0.007 (3)0.003 (3)
C150.039 (3)0.042 (3)0.063 (4)0.006 (2)0.008 (2)0.001 (2)
N110.040 (2)0.037 (2)0.045 (2)0.0022 (16)0.0006 (18)0.0015 (17)
C160.047 (3)0.043 (3)0.043 (3)0.004 (2)0.004 (2)0.003 (2)
N120.063 (3)0.066 (3)0.049 (3)0.002 (2)0.015 (2)0.002 (2)
C170.075 (4)0.067 (4)0.048 (3)0.003 (3)0.003 (3)0.009 (3)
C180.063 (4)0.053 (3)0.044 (3)0.004 (3)0.002 (2)0.003 (2)
N130.040 (2)0.036 (2)0.039 (2)0.0014 (16)0.0022 (17)0.0014 (16)
C190.049 (3)0.041 (3)0.042 (3)0.002 (2)0.000 (2)0.004 (2)
N140.090 (4)0.069 (3)0.044 (3)0.016 (3)0.004 (3)0.005 (2)
C200.101 (6)0.073 (4)0.042 (3)0.016 (4)0.003 (3)0.008 (3)
C210.060 (3)0.053 (3)0.049 (3)0.005 (3)0.003 (3)0.008 (3)
N150.0339 (19)0.0321 (19)0.048 (2)0.0005 (15)0.0031 (17)0.0007 (16)
C220.042 (3)0.039 (3)0.049 (3)0.001 (2)0.000 (2)0.009 (2)
N160.051 (3)0.047 (3)0.069 (3)0.014 (2)0.006 (2)0.011 (2)
C230.045 (3)0.048 (3)0.078 (4)0.012 (2)0.006 (3)0.005 (3)
C240.046 (3)0.038 (3)0.060 (3)0.008 (2)0.008 (2)0.001 (2)
N170.042 (2)0.037 (2)0.052 (3)0.0079 (17)0.0004 (19)0.0009 (19)
C250.075 (4)0.058 (3)0.060 (4)0.026 (3)0.009 (3)0.005 (3)
C260.094 (6)0.078 (5)0.083 (6)0.035 (4)0.032 (4)0.001 (4)
N180.080 (4)0.069 (4)0.087 (5)0.032 (3)0.010 (4)0.001 (3)
C270.072 (4)0.060 (4)0.072 (5)0.031 (3)0.007 (3)0.007 (3)
C280.052 (3)0.051 (3)0.056 (3)0.010 (3)0.003 (3)0.004 (3)
N190.0327 (19)0.0295 (18)0.046 (2)0.0030 (14)0.0027 (16)0.0020 (16)
C290.040 (2)0.035 (2)0.051 (3)0.0040 (19)0.013 (2)0.006 (2)
C300.039 (2)0.034 (2)0.048 (3)0.0020 (19)0.011 (2)0.005 (2)
Cl10.255 (4)0.0656 (13)0.136 (3)0.0206 (19)0.112 (3)0.0087 (14)
O10.217 (11)0.174 (10)0.265 (15)0.123 (9)0.011 (10)0.057 (10)
O20.51 (3)0.163 (10)0.187 (12)0.131 (13)0.222 (15)0.074 (8)
O30.354 (19)0.247 (14)0.103 (7)0.143 (14)0.059 (9)0.002 (8)
O40.209 (10)0.094 (5)0.189 (10)0.003 (6)0.085 (8)0.050 (6)
Cl20.0714 (11)0.1059 (15)0.0583 (10)0.0127 (10)0.0067 (8)0.0187 (10)
O50.318 (16)0.307 (16)0.142 (9)0.220 (15)0.070 (10)0.096 (10)
O60.122 (6)0.182 (8)0.063 (4)0.004 (5)0.009 (4)0.032 (4)
O70.333 (17)0.351 (18)0.116 (8)0.277 (16)0.003 (9)0.013 (9)
O80.102 (5)0.170 (7)0.066 (4)0.001 (5)0.024 (3)0.022 (4)
Cl30.0959 (15)0.1162 (18)0.0847 (15)0.0401 (14)0.0151 (12)0.0281 (13)
O90.217 (11)0.194 (10)0.153 (9)0.046 (9)0.044 (8)0.065 (8)
O100.094 (5)0.153 (7)0.102 (5)0.034 (4)0.004 (4)0.049 (5)
O110.127 (6)0.112 (5)0.133 (6)0.050 (5)0.030 (5)0.015 (5)
O120.122 (6)0.186 (9)0.175 (9)0.015 (6)0.052 (6)0.092 (7)
Si10.0410 (12)0.0498 (14)0.152 (3)0.0023 (10)0.0031 (16)0.0129 (17)
F10.077 (4)0.065 (3)0.447 (16)0.011 (3)0.063 (6)0.026 (6)
F20.076 (4)0.098 (4)0.340 (12)0.009 (3)0.064 (5)0.018 (6)
F30.224 (11)0.302 (15)0.203 (10)0.066 (10)0.083 (9)0.075 (10)
O1W0.178 (8)0.165 (8)0.104 (6)0.023 (7)0.020 (6)0.039 (6)
O2W0.134 (7)0.139 (7)0.163 (8)0.026 (5)0.050 (6)0.014 (6)
O3W0.120 (5)0.104 (5)0.086 (4)0.020 (4)0.016 (4)0.010 (4)
O4W0.243 (12)0.155 (8)0.174 (9)0.030 (8)0.116 (9)0.062 (7)
O5W0.16 (3)0.09 (2)0.20 (4)0.02 (2)0.06 (3)0.02 (2)
O6W0.35 (3)0.23 (2)0.125 (15)0.082 (19)0.004 (16)0.036 (15)
O7W0.27 (2)0.22 (2)0.42 (4)0.156 (19)0.13 (2)0.08 (2)
O8W0.27 (3)0.28 (3)0.33 (4)0.08 (2)0.01 (2)0.01 (2)
O9W0.22 (4)0.18 (3)0.19 (4)0.01 (3)0.05 (3)0.03 (2)
Geometric parameters (Å, º) top
Rh1—N72.053 (4)N12—C171.354 (9)
Rh1—N12.056 (4)N12—H12N0.8600
Rh1—N32.056 (5)C17—C181.367 (9)
Rh1—N52.056 (4)C17—H170.9300
Rh1—N172.238 (4)C18—H180.9300
Rh1—Rh22.6943 (5)N13—C191.327 (7)
Rh2—N132.044 (4)N13—C211.375 (7)
Rh2—N112.047 (4)C19—N141.335 (7)
Rh2—N92.048 (4)C19—C221.442 (8)
Rh2—N152.058 (4)N14—C201.373 (9)
Rh2—N192.251 (4)N14—H14N0.8600
N1—C11.345 (7)C20—C211.352 (9)
N1—C31.372 (7)C20—H200.9300
C1—N21.327 (8)C21—H210.9300
C1—C41.433 (9)N15—C221.329 (7)
N2—C21.363 (10)N15—C241.375 (7)
N2—H2N0.8600C22—N161.336 (7)
C2—C31.354 (9)N16—C231.356 (9)
C2—H20.9300N16—H16N0.8600
C3—H30.9300C23—C241.338 (8)
N3—C41.334 (7)C23—H230.9300
N3—C61.375 (8)C24—H240.9300
C4—N41.347 (8)N17—C251.331 (8)
N4—C51.346 (11)N17—C281.332 (7)
N4—H4N0.8600C25—C261.379 (9)
C5—C61.336 (11)C25—H250.9300
C5—H50.9300C26—N181.334 (10)
C6—H60.9300C26—H260.9300
N5—C71.335 (7)N18—C271.314 (10)
N5—C91.378 (8)C27—C281.376 (8)
C7—N61.338 (8)C27—H270.9300
C7—C101.429 (10)C28—H280.9300
N6—C81.337 (10)N19—C301.332 (6)
N6—H6N0.8600N19—C291.340 (6)
C8—C91.349 (9)C29—C30i1.370 (7)
C8—H80.9300C29—H290.9300
C9—H90.9300C30—C29i1.370 (7)
N7—C101.325 (9)C30—H300.9300
N7—C121.376 (8)Cl1—O11.358 (9)
C10—N81.347 (8)Cl1—O21.369 (11)
N8—C111.356 (12)Cl1—O41.403 (8)
N8—H8N0.8600Cl1—O31.460 (12)
C11—C121.350 (11)Cl2—O71.284 (9)
C11—H110.9300Cl2—O51.376 (11)
C12—H120.9300Cl2—O61.379 (7)
N9—C131.330 (7)Cl2—O81.386 (6)
N9—C151.379 (7)Cl3—O121.365 (8)
C13—N101.340 (7)Cl3—O101.388 (6)
C13—C161.430 (8)Cl3—O111.413 (7)
N10—C141.362 (9)Cl3—O91.483 (9)
N10—H10N0.8600Si1—F2ii1.625 (6)
C14—C151.346 (9)Si1—F21.625 (6)
C14—H140.9300Si1—F31.631 (9)
C15—H150.9300Si1—F3ii1.631 (9)
N11—C161.344 (7)Si1—F11.660 (6)
N11—C181.379 (7)Si1—F1ii1.660 (6)
C16—N121.334 (7)
N7—Rh1—N1175.44 (17)N9—C15—H15125.9
N7—Rh1—N3100.0 (2)C16—N11—C18106.2 (5)
N1—Rh1—N379.56 (18)C16—N11—Rh2113.8 (4)
N7—Rh1—N579.5 (2)C18—N11—Rh2139.4 (4)
N1—Rh1—N5100.68 (18)N12—C16—N11110.0 (5)
N3—Rh1—N5176.52 (16)N12—C16—C13134.3 (5)
N7—Rh1—N1788.62 (17)N11—C16—C13115.7 (5)
N1—Rh1—N1786.84 (16)C16—N12—C17108.6 (5)
N3—Rh1—N1789.94 (17)C16—N12—H12N125.7
N5—Rh1—N1786.61 (17)C17—N12—H12N125.7
N7—Rh1—Rh292.24 (12)N12—C17—C18106.9 (6)
N1—Rh1—Rh292.31 (11)N12—C17—H17126.5
N3—Rh1—Rh291.83 (12)C18—C17—H17126.5
N5—Rh1—Rh291.63 (12)C17—C18—N11108.2 (6)
N17—Rh1—Rh2177.87 (13)C17—C18—H18125.9
N13—Rh2—N11175.11 (16)N11—C18—H18125.9
N13—Rh2—N999.99 (17)C19—N13—C21106.0 (5)
N11—Rh2—N979.30 (17)C19—N13—Rh2113.8 (3)
N13—Rh2—N1579.47 (17)C21—N13—Rh2139.4 (4)
N11—Rh2—N15100.81 (17)N13—C19—N14111.3 (5)
N9—Rh2—N15175.04 (16)N13—C19—C22116.3 (5)
N13—Rh2—N1987.60 (16)N14—C19—C22132.4 (5)
N11—Rh2—N1987.54 (16)C19—N14—C20106.8 (5)
N9—Rh2—N1987.93 (15)C19—N14—H14N126.6
N15—Rh2—N1987.12 (15)C20—N14—H14N126.6
N13—Rh2—Rh192.36 (11)C21—C20—N14107.2 (6)
N11—Rh2—Rh192.50 (12)C21—C20—H20126.4
N9—Rh2—Rh192.30 (11)N14—C20—H20126.4
N15—Rh2—Rh192.65 (11)C20—C21—N13108.7 (5)
N19—Rh2—Rh1179.77 (10)C20—C21—H21125.7
C1—N1—C3105.6 (5)N13—C21—H21125.7
C1—N1—Rh1113.3 (4)C22—N15—C24106.2 (4)
C3—N1—Rh1140.5 (4)C22—N15—Rh2113.4 (3)
N2—C1—N1110.8 (6)C24—N15—Rh2140.4 (4)
N2—C1—C4133.0 (6)N15—C22—N16110.3 (5)
N1—C1—C4116.2 (5)N15—C22—C19116.4 (4)
C1—N2—C2107.5 (5)N16—C22—C19133.3 (5)
C1—N2—H2N126.2C22—N16—C23107.2 (5)
C2—N2—H2N126.2C22—N16—H16N126.4
C3—C2—N2107.2 (6)C23—N16—H16N126.4
C3—C2—H2126.4C24—C23—N16107.9 (5)
N2—C2—H2126.4C24—C23—H23126.1
C2—C3—N1108.8 (6)N16—C23—H23126.1
C2—C3—H3125.6C23—C24—N15108.4 (6)
N1—C3—H3125.6C23—C24—H24125.8
C4—N3—C6106.2 (5)N15—C24—H24125.8
C4—N3—Rh1113.4 (4)C25—N17—C28116.6 (5)
C6—N3—Rh1140.3 (5)C25—N17—Rh1122.6 (4)
N3—C4—N4110.1 (6)C28—N17—Rh1120.8 (4)
N3—C4—C1116.9 (5)N17—C25—C26120.9 (6)
N4—C4—C1132.9 (6)N17—C25—H25119.5
C5—N4—C4106.8 (6)C26—C25—H25119.5
C5—N4—H4N126.6N18—C26—C25122.7 (7)
C4—N4—H4N126.6N18—C26—H26118.7
C6—C5—N4108.8 (6)C25—C26—H26118.7
C6—C5—H5125.6C27—N18—C26115.5 (6)
N4—C5—H5125.6N18—C27—C28122.9 (6)
C5—C6—N3108.1 (7)N18—C27—H27118.6
C5—C6—H6126.0C28—C27—H27118.6
N3—C6—H6126.0N17—C28—C27121.4 (6)
C7—N5—C9106.7 (5)N17—C28—H28119.3
C7—N5—Rh1113.4 (4)C27—C28—H28119.3
C9—N5—Rh1139.8 (4)C30—N19—C29116.0 (4)
N5—C7—N6109.5 (6)C30—N19—Rh2122.0 (3)
N5—C7—C10116.0 (5)C29—N19—Rh2122.0 (3)
N6—C7—C10134.5 (6)N19—C29—C30i121.8 (5)
C8—N6—C7108.1 (5)N19—C29—H29119.1
C8—N6—H6N126.0C30i—C29—H29119.1
C7—N6—H6N126.0N19—C30—C29i122.2 (5)
N6—C8—C9108.3 (6)N19—C30—H30118.9
N6—C8—H8125.9C29i—C30—H30118.9
C9—C8—H8125.9O1—Cl1—O2109.3 (10)
C8—C9—N5107.5 (6)O1—Cl1—O4111.7 (8)
C8—C9—H9126.3O2—Cl1—O4106.4 (6)
N5—C9—H9126.3O1—Cl1—O3107.3 (8)
C10—N7—C12106.7 (6)O2—Cl1—O3112.9 (11)
C10—N7—Rh1113.0 (4)O4—Cl1—O3109.3 (8)
C12—N7—Rh1139.6 (5)O7—Cl2—O5109.2 (12)
N7—C10—N8110.4 (7)O7—Cl2—O6109.5 (7)
N7—C10—C7117.4 (5)O5—Cl2—O6108.6 (8)
N8—C10—C7132.2 (7)O7—Cl2—O8111.5 (7)
C10—N8—C11107.0 (7)O5—Cl2—O8103.0 (6)
C10—N8—H8N126.5O6—Cl2—O8114.7 (5)
C11—N8—H8N126.5O12—Cl3—O10114.3 (5)
C12—C11—N8108.0 (7)O12—Cl3—O11112.2 (6)
C12—C11—H11126.0O10—Cl3—O11112.4 (5)
N8—C11—H11126.0O12—Cl3—O9109.0 (8)
C11—C12—N7107.9 (8)O10—Cl3—O9104.5 (7)
C11—C12—H12126.0O11—Cl3—O9103.4 (7)
N7—C12—H12126.0F2ii—Si1—F2179.998 (2)
C13—N9—C15106.4 (4)F2ii—Si1—F389.5 (6)
C13—N9—Rh2113.9 (3)F2—Si1—F390.5 (6)
C15—N9—Rh2139.6 (4)F2ii—Si1—F3ii90.5 (6)
N9—C13—N10110.5 (5)F2—Si1—F3ii89.5 (6)
N9—C13—C16116.7 (5)F3—Si1—F3ii180.0 (7)
N10—C13—C16132.8 (5)F2ii—Si1—F193.7 (3)
C13—N10—C14107.1 (5)F2—Si1—F186.3 (3)
C13—N10—H10N126.5F3—Si1—F190.9 (6)
C14—N10—H10N126.5F3ii—Si1—F189.1 (6)
C15—C14—N10107.9 (5)F2ii—Si1—F1ii86.3 (3)
C15—C14—H14126.1F2—Si1—F1ii93.7 (3)
N10—C14—H14126.1F3—Si1—F1ii89.1 (6)
C14—C15—N9108.1 (6)F3ii—Si1—F1ii90.9 (6)
C14—C15—H15125.9F1—Si1—F1ii179.998 (1)
N7—Rh1—Rh2—N13118.86 (19)Rh1—Rh2—N9—C1397.6 (3)
N1—Rh1—Rh2—N1361.41 (17)N13—Rh2—N9—C154.9 (5)
N3—Rh1—Rh2—N13141.03 (18)N11—Rh2—N9—C15180.0 (6)
N5—Rh1—Rh2—N1339.35 (17)N15—Rh2—N9—C1588 (2)
N17—Rh1—Rh2—N135 (3)N19—Rh2—N9—C1592.1 (5)
N7—Rh1—Rh2—N1161.7 (2)Rh1—Rh2—N9—C1587.9 (5)
N1—Rh1—Rh2—N11118.08 (17)C15—N9—C13—N101.3 (6)
N3—Rh1—Rh2—N1138.46 (18)Rh2—N9—C13—N10177.6 (3)
N5—Rh1—Rh2—N11141.16 (17)C15—N9—C13—C16179.5 (5)
N17—Rh1—Rh2—N11175 (23)Rh2—N9—C13—C163.2 (6)
N7—Rh1—Rh2—N9141.0 (2)N9—C13—N10—C140.8 (6)
N1—Rh1—Rh2—N938.70 (18)C16—C13—N10—C14179.8 (6)
N3—Rh1—Rh2—N940.92 (18)C13—N10—C14—C150.0 (7)
N5—Rh1—Rh2—N9139.46 (18)N10—C14—C15—N90.8 (7)
N17—Rh1—Rh2—N9105 (3)C13—N9—C15—C141.3 (6)
N7—Rh1—Rh2—N1539.3 (2)Rh2—N9—C15—C14176.1 (4)
N1—Rh1—Rh2—N15140.97 (18)N13—Rh2—N11—C1675 (2)
N3—Rh1—Rh2—N15139.41 (18)N9—Rh2—N11—C167.0 (3)
N5—Rh1—Rh2—N1540.21 (18)N15—Rh2—N11—C16168.0 (3)
N17—Rh1—Rh2—N1574 (3)N19—Rh2—N11—C1681.4 (4)
N7—Rh1—Rh2—N1937 (27)Rh1—Rh2—N11—C1698.9 (3)
N1—Rh1—Rh2—N19144 (34)N13—Rh2—N11—C1894 (2)
N3—Rh1—Rh2—N19137 (34)N9—Rh2—N11—C18176.3 (6)
N5—Rh1—Rh2—N1943 (27)N15—Rh2—N11—C181.3 (6)
N17—Rh1—Rh2—N1977 (27)N19—Rh2—N11—C1887.9 (6)
N7—Rh1—N1—C178 (3)Rh1—Rh2—N11—C1891.8 (5)
N3—Rh1—N1—C17.0 (3)C18—N11—C16—N121.2 (6)
N5—Rh1—N1—C1169.4 (3)Rh2—N11—C16—N12174.0 (4)
N17—Rh1—N1—C183.5 (4)C18—N11—C16—C13179.8 (5)
Rh2—Rh1—N1—C198.5 (3)Rh2—N11—C16—C137.4 (6)
N7—Rh1—N1—C391 (3)N9—C13—C16—N12179.1 (6)
N3—Rh1—N1—C3176.4 (6)N10—C13—C16—N122.0 (11)
N5—Rh1—N1—C30.0 (6)N9—C13—C16—N112.8 (7)
N17—Rh1—N1—C385.9 (6)N10—C13—C16—N11176.1 (5)
Rh2—Rh1—N1—C392.1 (6)N11—C16—N12—C171.3 (7)
C3—N1—C1—N20.1 (6)C13—C16—N12—C17179.5 (6)
Rh1—N1—C1—N2173.1 (4)C16—N12—C17—C180.9 (7)
C3—N1—C1—C4179.9 (5)N12—C17—C18—N110.1 (7)
Rh1—N1—C1—C46.9 (6)C16—N11—C18—C170.7 (6)
N1—C1—N2—C20.8 (7)Rh2—N11—C18—C17170.5 (5)
C4—C1—N2—C2179.2 (6)N11—Rh2—N13—C1986 (2)
C1—N2—C2—C31.3 (7)N9—Rh2—N13—C19167.3 (4)
N2—C2—C3—N11.3 (7)N15—Rh2—N13—C197.7 (4)
C1—N1—C3—C20.9 (6)N19—Rh2—N13—C1979.9 (4)
Rh1—N1—C3—C2170.7 (5)Rh1—Rh2—N13—C1999.9 (3)
N7—Rh1—N3—C4169.3 (4)N11—Rh2—N13—C2182 (2)
N1—Rh1—N3—C46.1 (4)N9—Rh2—N13—C210.4 (6)
N5—Rh1—N3—C488 (3)N15—Rh2—N13—C21175.4 (6)
N17—Rh1—N3—C480.7 (4)N19—Rh2—N13—C2187.8 (6)
Rh2—Rh1—N3—C498.1 (4)Rh1—Rh2—N13—C2192.4 (6)
N7—Rh1—N3—C67.3 (6)C21—N13—C19—N140.2 (6)
N1—Rh1—N3—C6177.3 (6)Rh2—N13—C19—N14171.9 (4)
N5—Rh1—N3—C688 (3)C21—N13—C19—C22179.8 (5)
N17—Rh1—N3—C695.9 (6)Rh2—N13—C19—C228.5 (6)
Rh2—Rh1—N3—C685.3 (6)N13—C19—N14—C200.8 (8)
C6—N3—C4—N41.2 (6)C22—C19—N14—C20179.7 (6)
Rh1—N3—C4—N4178.9 (4)C19—N14—C20—C211.1 (9)
C6—N3—C4—C1177.9 (5)N14—C20—C21—N131.0 (9)
Rh1—N3—C4—C14.4 (6)C19—N13—C21—C200.5 (7)
N2—C1—C4—N3178.2 (6)Rh2—N13—C21—C20167.8 (5)
N1—C1—C4—N31.8 (7)N13—Rh2—N15—C225.6 (3)
N2—C1—C4—N45.9 (11)N11—Rh2—N15—C22169.5 (3)
N1—C1—C4—N4174.1 (6)N9—Rh2—N15—C2279 (2)
N3—C4—N4—C51.0 (7)N19—Rh2—N15—C2282.5 (4)
C1—C4—N4—C5177.1 (6)Rh1—Rh2—N15—C2297.5 (3)
C4—N4—C5—C60.4 (8)N13—Rh2—N15—C24178.6 (6)
N4—C5—C6—N30.3 (8)N11—Rh2—N15—C246.4 (6)
C4—N3—C6—C50.9 (7)N9—Rh2—N15—C2497 (2)
Rh1—N3—C6—C5177.6 (5)N19—Rh2—N15—C2493.3 (5)
N7—Rh1—N5—C75.9 (4)Rh1—Rh2—N15—C2486.7 (5)
N1—Rh1—N5—C7169.5 (4)C24—N15—C22—N160.4 (6)
N3—Rh1—N5—C776 (3)Rh2—N15—C22—N16177.6 (4)
N17—Rh1—N5—C783.3 (4)C24—N15—C22—C19179.9 (5)
Rh2—Rh1—N5—C797.9 (4)Rh2—N15—C22—C192.8 (6)
N7—Rh1—N5—C9179.5 (6)N13—C19—C22—N153.8 (7)
N1—Rh1—N5—C95.1 (6)N14—C19—C22—N15176.7 (6)
N3—Rh1—N5—C999 (3)N13—C19—C22—N16175.6 (6)
N17—Rh1—N5—C991.2 (6)N14—C19—C22—N163.9 (11)
Rh2—Rh1—N5—C987.6 (6)N15—C22—N16—C230.9 (7)
C9—N5—C7—N60.4 (6)C19—C22—N16—C23179.7 (6)
Rh1—N5—C7—N6176.7 (4)C22—N16—C23—C241.0 (7)
C9—N5—C7—C10179.8 (5)N16—C23—C24—N150.8 (7)
Rh1—N5—C7—C103.4 (6)C22—N15—C24—C230.3 (6)
N5—C7—N6—C80.4 (7)Rh2—N15—C24—C23175.7 (4)
C10—C7—N6—C8179.7 (6)N7—Rh1—N17—C2541.6 (5)
C7—N6—C8—C90.3 (8)N1—Rh1—N17—C25138.0 (5)
N6—C8—C9—N50.1 (7)N3—Rh1—N17—C2558.4 (5)
C7—N5—C9—C80.2 (6)N5—Rh1—N17—C25121.1 (5)
Rh1—N5—C9—C8175.0 (5)Rh2—Rh1—N17—C25155 (3)
N1—Rh1—N7—C1085 (3)N7—Rh1—N17—C28137.2 (5)
N3—Rh1—N7—C10168.9 (4)N1—Rh1—N17—C2843.3 (5)
N5—Rh1—N7—C107.6 (4)N3—Rh1—N17—C28122.8 (5)
N17—Rh1—N7—C1079.2 (4)N5—Rh1—N17—C2857.6 (5)
Rh2—Rh1—N7—C1098.8 (4)Rh2—Rh1—N17—C2823 (3)
N1—Rh1—N7—C1284 (3)C28—N17—C25—C260.3 (11)
N3—Rh1—N7—C120.8 (6)Rh1—N17—C25—C26179.1 (6)
N5—Rh1—N7—C12175.7 (6)N17—C25—C26—N180.7 (14)
N17—Rh1—N7—C1288.9 (6)C25—C26—N18—C270.7 (14)
Rh2—Rh1—N7—C1293.1 (6)C26—N18—C27—C280.3 (13)
C12—N7—C10—N81.6 (7)C25—N17—C28—C270.0 (10)
Rh1—N7—C10—N8173.6 (4)Rh1—N17—C28—C27178.8 (5)
C12—N7—C10—C7179.8 (5)N18—C27—C28—N170.0 (12)
Rh1—N7—C10—C78.2 (6)N13—Rh2—N19—C3045.3 (4)
N5—C7—C10—N73.3 (8)N11—Rh2—N19—C30134.2 (4)
N6—C7—C10—N7176.6 (6)N9—Rh2—N19—C3054.8 (4)
N5—C7—C10—N8179.1 (6)N15—Rh2—N19—C30124.9 (4)
N6—C7—C10—N81.1 (12)Rh1—Rh2—N19—C30128 (26)
N7—C10—N8—C111.8 (7)N13—Rh2—N19—C29134.8 (4)
C7—C10—N8—C11179.6 (6)N11—Rh2—N19—C2945.7 (4)
C10—N8—C11—C121.2 (8)N9—Rh2—N19—C29125.1 (4)
N8—C11—C12—N70.3 (8)N15—Rh2—N19—C2955.3 (4)
C10—N7—C12—C110.8 (7)Rh1—Rh2—N19—C2953 (27)
Rh1—N7—C12—C11169.4 (5)C30—N19—C29—C30i0.2 (9)
N13—Rh2—N9—C13169.6 (3)Rh2—N19—C29—C30i179.6 (4)
N11—Rh2—N9—C135.5 (3)C29—N19—C30—C29i0.2 (9)
N15—Rh2—N9—C1386 (2)Rh2—N19—C30—C29i179.6 (4)
N19—Rh2—N9—C1382.4 (4)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···F1iii0.861.992.767 (7)149
N4—H4N···O7W0.861.912.773 (17)176
N4—H4N···O5W0.862.032.73 (3)138
N6—H6N···F10.861.992.794 (8)156
N6—H6N···F20.862.343.056 (9)142
N8—H8N···F30.861.942.794 (11)170
N10—H10N···O3W0.862.022.841 (8)159
N12—H12N···O80.862.273.067 (9)154
N12—H12N···O100.862.422.965 (9)122
N14—H14N···O11i0.862.443.011 (10)125
N14—H14N···O20.862.543.058 (13)119
N16—H16N···O4W0.862.042.856 (10)158
N16—H16N···O11i0.862.623.131 (10)120
Symmetry codes: (i) x+1, y+1, z+1; (iii) x+1/2, y+3/2, z+1.
(VII) top
Crystal data top
C60H60N38Rh4·8(ClO4)·11.41(H2O)Dx = 1.847 Mg m3
Mr = 2726.26Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, PbcaCell parameters from 19919 reflections
a = 20.289 (4) Åθ = 3.1–27.5°
b = 21.524 (5) ŵ = 0.99 mm1
c = 22.450 (5) ÅT = 296 K
V = 9804 (4) Å3Prismatic, red
Z = 40.42 × 0.35 × 0.25 mm
F(000) = 5488
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
11220 independent reflections
Radiation source: rotating-anode X-ray tube8509 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.104
Detector resolution: 14.6306 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = 2526
Absorption correction: numerical
NUMABS (Higashi, 1999)
k = 1727
Tmin = 0.807, Tmax = 0.884l = 2929
72426 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.092Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.231H atoms treated by a mixture of independent and constrained refinement
S = 1.15 w = 1/[σ2(Fo2) + (0.0905P)2 + 33.6829P]
where P = (Fo2 + 2Fc2)/3
11220 reflections(Δ/σ)max = 0.001
706 parametersΔρmax = 1.49 e Å3
19 restraintsΔρmin = 1.06 e Å3
Crystal data top
C60H60N38Rh4·8(ClO4)·11.41(H2O)V = 9804 (4) Å3
Mr = 2726.26Z = 4
Orthorhombic, PbcaMo Kα radiation
a = 20.289 (4) ŵ = 0.99 mm1
b = 21.524 (5) ÅT = 296 K
c = 22.450 (5) Å0.42 × 0.35 × 0.25 mm
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
11220 independent reflections
Absorption correction: numerical
NUMABS (Higashi, 1999)
8509 reflections with I > 2σ(I)
Tmin = 0.807, Tmax = 0.884Rint = 0.104
72426 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.09219 restraints
wR(F2) = 0.231H atoms treated by a mixture of independent and constrained refinement
S = 1.15 w = 1/[σ2(Fo2) + (0.0905P)2 + 33.6829P]
where P = (Fo2 + 2Fc2)/3
11220 reflectionsΔρmax = 1.49 e Å3
706 parametersΔρmin = 1.06 e Å3
Special details top

Experimental. ????

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 not 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
xyzUiso*/UeqOcc. (<1)
Rh10.28661 (3)0.70345 (3)0.56605 (2)0.03821 (17)
Rh20.37753 (3)0.61688 (2)0.53858 (2)0.03527 (16)
N10.3341 (3)0.7707 (3)0.5160 (3)0.0470 (15)
C10.3720 (4)0.8078 (4)0.5485 (4)0.056 (2)
N20.3962 (4)0.8542 (3)0.5151 (4)0.069 (2)
H2N0.42110.88390.52720.083*
C20.3738 (5)0.8453 (4)0.4581 (5)0.070 (3)
H20.38320.86980.42500.085*
C30.3359 (4)0.7950 (4)0.4595 (4)0.056 (2)
H30.31370.77860.42690.067*
N30.3474 (3)0.7431 (3)0.6295 (3)0.0490 (15)
C40.3805 (4)0.7923 (4)0.6101 (4)0.058 (2)
N40.4179 (4)0.8155 (4)0.6541 (4)0.075 (2)
H4N0.44410.84690.65180.090*
C50.4067 (6)0.7801 (6)0.7024 (5)0.084 (3)
H50.42590.78560.73970.101*
C60.3633 (5)0.7357 (5)0.6880 (4)0.067 (3)
H60.34690.70520.71340.081*
N50.2218 (3)0.6667 (3)0.5047 (3)0.0408 (13)
C70.1783 (4)0.6287 (4)0.5302 (4)0.0507 (19)
N60.1350 (4)0.6086 (4)0.4889 (4)0.063 (2)
H6N0.10200.58430.49500.076*
C80.1532 (5)0.6340 (5)0.4357 (5)0.066 (3)
H80.13270.62710.39930.080*
C90.2064 (4)0.6710 (4)0.4450 (4)0.055 (2)
H90.22820.69470.41660.065*
N70.2356 (3)0.6428 (3)0.6188 (3)0.0467 (15)
C100.1848 (4)0.6171 (3)0.5927 (4)0.0485 (18)
N80.1505 (4)0.5832 (4)0.6319 (4)0.065 (2)
H8N0.11640.56090.62400.078*
C110.1791 (5)0.5902 (5)0.6865 (4)0.068 (3)
H110.16480.57360.72240.082*
C120.2316 (5)0.6258 (4)0.6776 (4)0.063 (2)
H120.26150.63750.70690.075*
N90.4530 (3)0.6796 (3)0.5470 (3)0.0398 (13)
C130.4828 (4)0.6769 (4)0.5995 (4)0.0489 (18)
N100.5329 (3)0.7177 (3)0.6013 (3)0.0581 (18)
H10N0.55830.72510.63110.070*
C140.5356 (4)0.7451 (4)0.5460 (4)0.063 (2)
H140.56560.77520.53400.076*
C150.4881 (4)0.7213 (3)0.5132 (4)0.0519 (19)
H150.47970.73120.47360.062*
N110.4022 (3)0.6039 (3)0.6265 (3)0.0423 (14)
C160.4560 (4)0.6349 (3)0.6425 (3)0.0439 (17)
N120.4732 (4)0.6189 (4)0.6979 (3)0.064 (2)
H12N0.50580.63360.71790.077*
C170.4302 (5)0.5754 (4)0.7169 (4)0.064 (2)
H170.43090.55540.75360.076*
C180.3861 (4)0.5661 (4)0.6727 (3)0.0526 (19)
H180.35080.53850.67370.063*
N130.3591 (3)0.6256 (3)0.4492 (3)0.0412 (13)
C190.3220 (4)0.5800 (4)0.4277 (3)0.0471 (17)
N140.3204 (4)0.5829 (4)0.3681 (3)0.065 (2)
H14N0.29930.55820.34480.078*
C200.3580 (6)0.6318 (5)0.3510 (4)0.073 (3)
H200.36570.64510.31220.088*
C210.3821 (4)0.6571 (4)0.4014 (4)0.055 (2)
H210.41040.69110.40310.066*
N150.3074 (3)0.5487 (3)0.5275 (3)0.0393 (13)
C220.2913 (4)0.5394 (3)0.4711 (4)0.0447 (17)
N160.2485 (4)0.4928 (3)0.4661 (3)0.0596 (18)
H16N0.23110.47960.43350.072*
C230.2372 (5)0.4700 (4)0.5209 (4)0.062 (2)
H230.21020.43660.53060.074*
C240.2732 (4)0.5052 (4)0.5594 (4)0.0519 (19)
H240.27440.50050.60060.062*
N170.2086 (3)0.7745 (3)0.5835 (3)0.0459 (14)
C250.1804 (5)0.7835 (4)0.6359 (4)0.060 (2)
H250.19380.76000.66840.072*
C260.1315 (6)0.8271 (5)0.6430 (5)0.081 (3)
H260.11350.83230.68070.097*
N180.1088 (4)0.8620 (4)0.5992 (4)0.075 (2)
C270.1375 (5)0.8526 (4)0.5473 (4)0.063 (2)
H270.12390.87590.51470.076*
C280.1870 (4)0.8094 (4)0.5397 (4)0.057 (2)
H280.20570.80490.50210.068*
N190.4529 (3)0.5445 (3)0.5144 (3)0.0393 (13)
C290.4577 (4)0.4910 (3)0.5438 (3)0.0413 (16)
H290.42870.48320.57500.050*
C300.4959 (4)0.5532 (3)0.4705 (3)0.0445 (17)
H300.49460.59010.44890.053*
Cl10.2784 (2)0.58212 (17)0.20406 (19)0.1286 (15)
O10.2231 (7)0.5460 (6)0.2042 (7)0.187 (6)
O20.3295 (8)0.5535 (5)0.2354 (6)0.193 (7)
O30.2972 (8)0.5916 (7)0.1422 (5)0.198 (7)
O40.2645 (7)0.6403 (4)0.2322 (5)0.165 (5)
Cl20.50756 (14)0.69240 (14)0.84318 (12)0.0789 (7)
O50.4635 (8)0.6450 (8)0.8381 (6)0.220 (8)
O60.5378 (5)0.6906 (6)0.8985 (4)0.137 (4)
O70.4742 (8)0.7450 (7)0.8379 (5)0.217 (8)
O80.5518 (4)0.6851 (5)0.7955 (4)0.111 (3)
Cl30.64676 (16)0.59659 (16)0.63272 (13)0.0886 (9)
O90.6855 (6)0.6403 (6)0.5983 (5)0.158 (5)
O100.6163 (4)0.6302 (4)0.6793 (4)0.104 (3)
O110.6923 (5)0.5536 (4)0.6566 (4)0.125 (3)
O120.6007 (5)0.5672 (5)0.5943 (5)0.140 (4)
Cl40.00139 (18)0.48605 (18)0.59243 (19)0.1097 (11)
O130.0592 (5)0.5080 (6)0.5705 (7)0.178 (6)
O140.0024 (5)0.4208 (4)0.5774 (6)0.152 (5)
O150.0519 (6)0.5168 (7)0.5621 (6)0.191 (6)
O160.0074 (9)0.4967 (7)0.6545 (6)0.214 (7)
O1W0.3173 (6)0.8456 (6)0.3115 (4)0.142 (4)
O2W0.2372 (6)0.7423 (6)0.3120 (5)0.156 (4)
O3W0.5991 (5)0.7671 (4)0.7013 (4)0.119 (3)
O4W0.1792 (6)0.4799 (7)0.3533 (6)0.190 (6)
O5W0.523 (2)0.8785 (19)0.702 (3)0.18 (2)0.30 (3)
O6W0.6142 (17)0.9137 (13)0.7117 (11)0.277 (18)0.70 (3)
O7W0.4892 (16)0.9167 (16)0.770 (2)0.34 (2)0.70 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0368 (3)0.0390 (3)0.0388 (3)0.0020 (2)0.0010 (2)0.0019 (2)
Rh20.0337 (3)0.0343 (3)0.0378 (3)0.0003 (2)0.0013 (2)0.0016 (2)
N10.045 (4)0.041 (3)0.055 (4)0.000 (3)0.005 (3)0.002 (3)
C10.045 (4)0.046 (4)0.076 (6)0.010 (4)0.005 (4)0.003 (4)
N20.061 (5)0.041 (4)0.105 (7)0.007 (3)0.017 (5)0.005 (4)
C20.067 (6)0.053 (5)0.091 (8)0.006 (4)0.022 (6)0.002 (5)
C30.057 (5)0.052 (5)0.060 (5)0.001 (4)0.008 (4)0.005 (4)
N30.044 (3)0.053 (4)0.050 (4)0.004 (3)0.005 (3)0.015 (3)
C40.047 (5)0.051 (5)0.076 (6)0.006 (4)0.011 (4)0.020 (4)
N40.069 (5)0.071 (5)0.084 (6)0.001 (4)0.018 (5)0.030 (5)
C50.079 (7)0.101 (8)0.072 (7)0.016 (6)0.019 (6)0.042 (7)
C60.063 (6)0.085 (7)0.053 (5)0.019 (5)0.007 (4)0.018 (5)
N50.042 (3)0.039 (3)0.042 (3)0.002 (3)0.001 (3)0.002 (3)
C70.037 (4)0.047 (4)0.068 (5)0.003 (3)0.002 (4)0.018 (4)
N60.051 (4)0.063 (5)0.076 (5)0.007 (3)0.009 (4)0.012 (4)
C80.053 (5)0.075 (6)0.072 (6)0.018 (5)0.023 (5)0.024 (5)
C90.058 (5)0.051 (5)0.054 (5)0.015 (4)0.009 (4)0.003 (4)
N70.052 (4)0.047 (4)0.041 (3)0.010 (3)0.008 (3)0.002 (3)
C100.045 (4)0.040 (4)0.061 (5)0.008 (3)0.009 (4)0.004 (4)
N80.049 (4)0.063 (5)0.082 (6)0.003 (3)0.023 (4)0.006 (4)
C110.078 (7)0.081 (7)0.046 (5)0.016 (5)0.021 (5)0.016 (5)
C120.078 (6)0.058 (5)0.052 (5)0.013 (5)0.013 (5)0.009 (4)
N90.039 (3)0.031 (3)0.049 (3)0.005 (2)0.000 (3)0.002 (2)
C130.047 (4)0.049 (4)0.050 (4)0.003 (3)0.005 (4)0.009 (4)
N100.046 (4)0.064 (4)0.064 (5)0.002 (3)0.012 (3)0.016 (4)
C140.051 (5)0.052 (5)0.086 (7)0.010 (4)0.010 (5)0.005 (5)
C150.046 (4)0.039 (4)0.070 (5)0.004 (3)0.009 (4)0.000 (4)
N110.046 (3)0.041 (3)0.040 (3)0.000 (3)0.002 (3)0.005 (3)
C160.035 (4)0.048 (4)0.048 (4)0.009 (3)0.004 (3)0.011 (3)
N120.056 (4)0.077 (5)0.060 (4)0.005 (4)0.018 (4)0.008 (4)
C170.080 (6)0.062 (5)0.049 (5)0.002 (5)0.004 (5)0.001 (4)
C180.055 (5)0.058 (5)0.045 (4)0.001 (4)0.004 (4)0.001 (4)
N130.039 (3)0.043 (3)0.041 (3)0.002 (3)0.004 (3)0.003 (3)
C190.047 (4)0.052 (4)0.043 (4)0.008 (3)0.003 (3)0.004 (3)
N140.079 (5)0.071 (5)0.045 (4)0.018 (4)0.005 (4)0.007 (4)
C200.096 (8)0.072 (6)0.052 (5)0.020 (6)0.001 (5)0.014 (5)
C210.058 (5)0.060 (5)0.048 (4)0.003 (4)0.002 (4)0.009 (4)
N150.035 (3)0.041 (3)0.041 (3)0.002 (2)0.005 (2)0.001 (3)
C220.041 (4)0.035 (4)0.058 (5)0.001 (3)0.004 (3)0.012 (3)
N160.055 (4)0.056 (4)0.068 (5)0.017 (3)0.007 (4)0.018 (4)
C230.060 (5)0.053 (5)0.072 (6)0.021 (4)0.012 (5)0.005 (4)
C240.042 (4)0.053 (5)0.060 (5)0.004 (3)0.013 (4)0.004 (4)
N170.039 (3)0.042 (3)0.056 (4)0.007 (3)0.004 (3)0.000 (3)
C250.063 (5)0.058 (5)0.060 (5)0.024 (4)0.005 (4)0.003 (4)
C260.097 (8)0.083 (7)0.064 (6)0.024 (6)0.027 (6)0.003 (5)
N180.083 (6)0.071 (5)0.071 (5)0.035 (4)0.010 (4)0.006 (4)
C270.073 (6)0.058 (5)0.059 (5)0.026 (5)0.008 (5)0.011 (4)
C280.052 (5)0.065 (5)0.053 (5)0.014 (4)0.002 (4)0.003 (4)
N190.040 (3)0.033 (3)0.044 (3)0.001 (2)0.005 (3)0.001 (2)
C290.043 (4)0.041 (4)0.040 (4)0.007 (3)0.008 (3)0.006 (3)
C300.042 (4)0.036 (4)0.055 (4)0.007 (3)0.003 (3)0.008 (3)
Cl10.189 (4)0.079 (2)0.118 (3)0.028 (2)0.069 (3)0.004 (2)
O10.190 (12)0.153 (11)0.219 (14)0.105 (10)0.013 (10)0.046 (10)
O20.303 (18)0.129 (9)0.147 (10)0.042 (11)0.126 (12)0.020 (8)
O30.308 (18)0.201 (13)0.085 (7)0.123 (13)0.023 (9)0.010 (8)
O40.251 (13)0.068 (5)0.177 (11)0.004 (7)0.120 (10)0.037 (6)
Cl20.0708 (16)0.099 (2)0.0673 (15)0.0153 (14)0.0043 (12)0.0202 (14)
O50.260 (17)0.245 (16)0.154 (11)0.161 (15)0.061 (11)0.075 (11)
O60.131 (8)0.215 (12)0.065 (5)0.030 (8)0.015 (5)0.040 (6)
O70.299 (18)0.232 (15)0.120 (9)0.196 (15)0.014 (10)0.000 (9)
O80.091 (6)0.167 (9)0.075 (5)0.020 (6)0.024 (5)0.016 (5)
Cl30.090 (2)0.103 (2)0.0733 (17)0.0298 (17)0.0069 (15)0.0128 (16)
O90.157 (10)0.180 (11)0.136 (9)0.052 (9)0.016 (8)0.050 (9)
O100.084 (5)0.152 (8)0.076 (5)0.048 (5)0.000 (4)0.032 (5)
O110.155 (9)0.103 (7)0.117 (7)0.061 (6)0.032 (6)0.019 (6)
O120.122 (8)0.179 (11)0.119 (8)0.001 (7)0.045 (6)0.061 (8)
Cl40.093 (2)0.109 (3)0.128 (3)0.013 (2)0.006 (2)0.034 (2)
O130.091 (8)0.150 (10)0.293 (17)0.043 (7)0.045 (9)0.057 (11)
O140.101 (7)0.078 (6)0.277 (15)0.003 (5)0.031 (8)0.048 (8)
O150.149 (11)0.220 (14)0.202 (13)0.125 (10)0.049 (9)0.019 (10)
O160.32 (2)0.222 (15)0.097 (8)0.027 (15)0.015 (11)0.050 (9)
O1W0.162 (10)0.171 (10)0.094 (7)0.000 (8)0.006 (7)0.023 (7)
O2W0.133 (10)0.170 (11)0.165 (11)0.029 (8)0.026 (8)0.018 (9)
O3W0.135 (8)0.115 (7)0.108 (7)0.020 (6)0.019 (6)0.038 (6)
O4W0.152 (11)0.260 (15)0.159 (11)0.061 (11)0.066 (9)0.104 (11)
O5W0.18 (4)0.14 (3)0.23 (4)0.11 (3)0.06 (3)0.02 (3)
O6W0.42 (4)0.26 (3)0.150 (19)0.14 (3)0.02 (2)0.012 (18)
O7W0.29 (3)0.28 (3)0.44 (4)0.10 (2)0.08 (3)0.13 (3)
Geometric parameters (Å, º) top
Rh1—N72.043 (6)C16—N121.337 (10)
Rh1—N52.062 (6)N12—C171.348 (11)
Rh1—N32.069 (6)N12—H12N0.8600
Rh1—N12.071 (6)C17—C181.352 (12)
Rh1—N172.235 (6)C17—H170.9300
Rh1—Rh22.6935 (8)C18—H180.9300
Rh2—N132.049 (6)N13—C191.327 (9)
Rh2—N92.050 (6)N13—C211.354 (10)
Rh2—N112.056 (6)C19—N141.341 (10)
Rh2—N152.059 (6)C19—C221.449 (11)
Rh2—N192.248 (6)N14—C201.354 (12)
N1—C11.327 (11)N14—H14N0.8600
N1—C31.372 (10)C20—C211.348 (13)
C1—N21.341 (11)C20—H200.9300
C1—C41.434 (13)C21—H210.9300
N2—C21.371 (13)N15—C221.323 (9)
N2—H2N0.8600N15—C241.367 (10)
C2—C31.329 (13)C22—N161.332 (9)
C2—H20.9300N16—C231.343 (11)
C3—H30.9300N16—H16N0.8600
N3—C41.328 (11)C23—C241.364 (12)
N3—C61.361 (11)C23—H230.9300
C4—N41.341 (11)C24—H240.9300
N4—C51.345 (14)N17—C281.314 (10)
N4—H4N0.8600N17—C251.323 (10)
C5—C61.341 (15)C25—C261.374 (13)
C5—H50.9300C25—H250.9300
C6—H60.9300C26—N181.320 (13)
N5—C71.334 (10)C26—H260.9300
N5—C91.379 (10)N18—C271.319 (11)
C7—N61.347 (10)C27—C281.379 (12)
C7—C101.432 (12)C27—H270.9300
N6—C81.364 (13)C28—H280.9300
N6—H6N0.8600N19—C301.331 (9)
C8—C91.356 (13)N19—C291.331 (9)
C8—H80.9300C29—C30i1.378 (10)
C9—H90.9300C29—H290.9300
N7—C101.308 (10)C30—C29i1.378 (10)
N7—C121.372 (10)C30—H300.9300
C10—N81.339 (10)Cl1—O11.365 (11)
N8—C111.365 (12)Cl1—O21.396 (12)
N8—H8N0.8600Cl1—O41.431 (10)
C11—C121.327 (13)Cl1—O31.454 (12)
C11—H110.9300Cl2—O71.324 (11)
C12—H120.9300Cl2—O51.361 (12)
N9—C131.325 (10)Cl2—O61.385 (9)
N9—C151.375 (10)Cl2—O81.406 (8)
C13—N101.344 (10)Cl3—O101.413 (8)
C13—C161.430 (11)Cl3—O111.413 (9)
N10—C141.374 (12)Cl3—O121.421 (9)
N10—H10N0.8600Cl3—O91.449 (10)
C14—C151.316 (12)Cl4—O151.396 (10)
C14—H140.9300Cl4—O131.406 (11)
C15—H150.9300Cl4—O161.418 (12)
N11—C161.329 (9)Cl4—O141.444 (9)
N11—C181.357 (10)
N7—Rh1—N579.6 (3)C15—C14—H14126.0
N7—Rh1—N399.6 (3)N10—C14—H14126.0
N5—Rh1—N3176.9 (2)C14—C15—N9108.9 (8)
N7—Rh1—N1175.3 (2)C14—C15—H15125.5
N5—Rh1—N1101.7 (3)N9—C15—H15125.5
N3—Rh1—N178.9 (3)C16—N11—C18107.0 (7)
N7—Rh1—N1788.7 (2)C16—N11—Rh2113.0 (5)
N5—Rh1—N1785.9 (2)C18—N11—Rh2139.1 (5)
N3—Rh1—N1791.1 (2)N11—C16—N12109.6 (7)
N1—Rh1—N1786.9 (2)N11—C16—C13116.6 (7)
N7—Rh1—Rh292.15 (17)N12—C16—C13133.8 (7)
N5—Rh1—Rh291.04 (16)C16—N12—C17107.8 (7)
N3—Rh1—Rh291.96 (18)C16—N12—H12N126.1
N1—Rh1—Rh292.34 (17)C17—N12—H12N126.1
N17—Rh1—Rh2176.61 (17)N12—C17—C18107.4 (8)
N13—Rh2—N999.6 (2)N12—C17—H17126.3
N13—Rh2—N11175.6 (2)C18—C17—H17126.3
N9—Rh2—N1179.6 (2)C17—C18—N11108.2 (8)
N13—Rh2—N1579.7 (2)C17—C18—H18125.9
N9—Rh2—N15175.2 (2)N11—C18—H18125.9
N11—Rh2—N15100.8 (2)C19—N13—C21106.2 (7)
N13—Rh2—N1987.2 (2)C19—N13—Rh2113.1 (5)
N9—Rh2—N1988.3 (2)C21—N13—Rh2139.3 (6)
N11—Rh2—N1988.4 (2)N13—C19—N14110.0 (7)
N15—Rh2—N1987.0 (2)N13—C19—C22116.3 (6)
N13—Rh2—Rh192.05 (17)N14—C19—C22133.7 (7)
N9—Rh2—Rh192.01 (16)C19—N14—C20107.8 (7)
N11—Rh2—Rh192.33 (17)C19—N14—H14N126.1
N15—Rh2—Rh192.72 (16)C20—N14—H14N126.1
N19—Rh2—Rh1179.23 (16)C21—C20—N14106.3 (8)
C1—N1—C3105.3 (7)C21—C20—H20126.9
C1—N1—Rh1113.1 (6)N14—C20—H20126.9
C3—N1—Rh1141.2 (6)C20—C21—N13109.7 (8)
N1—C1—N2110.6 (9)C20—C21—H21125.1
N1—C1—C4117.4 (8)N13—C21—H21125.1
N2—C1—C4132.0 (9)C22—N15—C24105.9 (6)
C1—N2—C2107.3 (8)C22—N15—Rh2113.1 (5)
C1—N2—H2N126.3C24—N15—Rh2140.8 (6)
C2—N2—H2N126.3N15—C22—N16110.8 (7)
C3—C2—N2106.4 (9)N15—C22—C19116.6 (6)
C3—C2—H2126.8N16—C22—C19132.6 (7)
N2—C2—H2126.8C22—N16—C23108.0 (7)
C2—C3—N1110.3 (9)C22—N16—H16N126.0
C2—C3—H3124.8C23—N16—H16N126.0
N1—C3—H3124.8N16—C23—C24106.6 (7)
C4—N3—C6106.9 (8)N16—C23—H23126.7
C4—N3—Rh1113.9 (6)C24—C23—H23126.7
C6—N3—Rh1139.2 (7)C23—C24—N15108.7 (8)
N3—C4—N4110.0 (9)C23—C24—H24125.7
N3—C4—C1116.2 (7)N15—C24—H24125.7
N4—C4—C1133.7 (10)C28—N17—C25115.9 (7)
C4—N4—C5106.7 (9)C28—N17—Rh1119.8 (6)
C4—N4—H4N126.6C25—N17—Rh1124.3 (5)
C5—N4—H4N126.6N17—C25—C26121.1 (8)
C6—C5—N4108.7 (9)N17—C25—H25119.5
C6—C5—H5125.7C26—C25—H25119.5
N4—C5—H5125.7N18—C26—C25123.7 (9)
C5—C6—N3107.8 (10)N18—C26—H26118.2
C5—C6—H6126.1C25—C26—H26118.2
N3—C6—H6126.1C27—N18—C26114.6 (8)
C7—N5—C9107.9 (7)N18—C27—C28122.4 (9)
C7—N5—Rh1111.8 (5)N18—C27—H27118.8
C9—N5—Rh1140.3 (6)C28—C27—H27118.8
N5—C7—N6109.5 (8)N17—C28—C27122.4 (8)
N5—C7—C10117.8 (7)N17—C28—H28118.8
N6—C7—C10132.8 (8)C27—C28—H28118.8
C7—N6—C8107.3 (8)C30—N19—C29116.2 (6)
C7—N6—H6N126.3C30—N19—Rh2121.8 (5)
C8—N6—H6N126.3C29—N19—Rh2122.0 (5)
C9—C8—N6108.4 (8)N19—C29—C30i122.2 (7)
C9—C8—H8125.8N19—C29—H29118.9
N6—C8—H8125.8C30i—C29—H29118.9
C8—C9—N5107.0 (8)N19—C30—C29i121.6 (7)
C8—C9—H9126.5N19—C30—H30119.2
N5—C9—H9126.5C29i—C30—H30119.2
C10—N7—C12105.7 (7)O1—Cl1—O2111.0 (10)
C10—N7—Rh1114.2 (5)O1—Cl1—O4109.6 (9)
C12—N7—Rh1139.3 (6)O2—Cl1—O4108.0 (7)
N7—C10—N8110.3 (8)O1—Cl1—O3107.3 (8)
N7—C10—C7116.0 (7)O2—Cl1—O3110.4 (10)
N8—C10—C7133.7 (8)O4—Cl1—O3110.5 (8)
C10—N8—C11107.9 (8)O7—Cl2—O5107.2 (12)
C10—N8—H8N126.1O7—Cl2—O6109.3 (8)
C11—N8—H8N126.1O5—Cl2—O6110.2 (9)
C12—C11—N8105.7 (8)O7—Cl2—O8110.8 (8)
C12—C11—H11127.1O5—Cl2—O8105.7 (7)
N8—C11—H11127.1O6—Cl2—O8113.4 (6)
C11—C12—N7110.3 (9)O10—Cl3—O11109.9 (6)
C11—C12—H12124.9O10—Cl3—O12113.0 (6)
N7—C12—H12124.9O11—Cl3—O12111.6 (7)
C13—N9—C15106.4 (7)O10—Cl3—O9107.3 (7)
C13—N9—Rh2113.2 (5)O11—Cl3—O9105.9 (8)
C15—N9—Rh2140.0 (6)O12—Cl3—O9108.8 (7)
N9—C13—N10110.1 (7)O15—Cl4—O13108.2 (10)
N9—C13—C16117.0 (7)O15—Cl4—O16109.8 (10)
N10—C13—C16132.9 (8)O13—Cl4—O16111.4 (10)
C13—N10—C14106.5 (7)O15—Cl4—O14109.6 (8)
C13—N10—H10N126.8O13—Cl4—O14105.0 (7)
C14—N10—H10N126.8O16—Cl4—O14112.6 (10)
C15—C14—N10108.0 (8)
N7—Rh1—Rh2—N13122.2 (3)Rh1—Rh2—N9—C1397.9 (5)
N5—Rh1—Rh2—N1342.5 (2)N13—Rh2—N9—C152.3 (8)
N3—Rh1—Rh2—N13138.2 (3)N11—Rh2—N9—C15177.8 (8)
N1—Rh1—Rh2—N1359.2 (3)N15—Rh2—N9—C1583 (3)
N17—Rh1—Rh2—N1318 (3)N19—Rh2—N9—C1589.1 (8)
N7—Rh1—Rh2—N9138.1 (3)Rh1—Rh2—N9—C1590.2 (8)
N5—Rh1—Rh2—N9142.2 (2)C15—N9—C13—N103.4 (9)
N3—Rh1—Rh2—N938.5 (3)Rh2—N9—C13—N10178.0 (5)
N1—Rh1—Rh2—N940.5 (2)C15—N9—C13—C16178.6 (7)
N17—Rh1—Rh2—N9118 (3)Rh2—N9—C13—C164.0 (9)
N7—Rh1—Rh2—N1158.5 (3)N9—C13—N10—C142.4 (9)
N5—Rh1—Rh2—N11138.1 (2)C16—C13—N10—C14180.0 (9)
N3—Rh1—Rh2—N1141.2 (3)C13—N10—C14—C150.4 (10)
N1—Rh1—Rh2—N11120.1 (3)N10—C14—C15—N91.6 (10)
N17—Rh1—Rh2—N11163 (3)C13—N9—C15—C143.1 (9)
N7—Rh1—Rh2—N1542.4 (2)Rh2—N9—C15—C14175.4 (6)
N5—Rh1—Rh2—N1537.2 (2)N13—Rh2—N11—C1673 (3)
N3—Rh1—Rh2—N15142.1 (3)N9—Rh2—N11—C166.9 (5)
N1—Rh1—Rh2—N15139.0 (2)N15—Rh2—N11—C16168.2 (5)
N17—Rh1—Rh2—N1562 (3)N19—Rh2—N11—C1681.6 (5)
N7—Rh1—Rh2—N19107 (11)Rh1—Rh2—N11—C1698.6 (5)
N5—Rh1—Rh2—N1927 (11)N13—Rh2—N11—C1894 (3)
N3—Rh1—Rh2—N19153 (11)N9—Rh2—N11—C18174.5 (8)
N1—Rh1—Rh2—N1974 (11)N15—Rh2—N11—C180.7 (8)
N17—Rh1—Rh2—N193 (12)N19—Rh2—N11—C1885.9 (8)
N7—Rh1—N1—C165 (3)Rh1—Rh2—N11—C1893.9 (8)
N5—Rh1—N1—C1170.4 (5)C18—N11—C16—N121.5 (8)
N3—Rh1—N1—C16.5 (5)Rh2—N11—C16—N12173.0 (5)
N17—Rh1—N1—C185.3 (6)C18—N11—C16—C13178.5 (7)
Rh2—Rh1—N1—C198.0 (5)Rh2—N11—C16—C137.0 (8)
N7—Rh1—N1—C3107 (3)N9—C13—C16—N112.1 (10)
N5—Rh1—N1—C31.3 (9)N10—C13—C16—N11175.3 (8)
N3—Rh1—N1—C3178.2 (9)N9—C13—C16—N12178.0 (8)
N17—Rh1—N1—C386.5 (9)N10—C13—C16—N124.6 (16)
Rh2—Rh1—N1—C390.2 (9)N11—C16—N12—C171.6 (9)
C3—N1—C1—N21.0 (9)C13—C16—N12—C17178.4 (8)
Rh1—N1—C1—N2173.7 (5)C16—N12—C17—C181.1 (10)
C3—N1—C1—C4178.6 (7)N12—C17—C18—N110.1 (10)
Rh1—N1—C1—C46.8 (9)C16—N11—C18—C170.9 (9)
N1—C1—N2—C21.5 (10)Rh2—N11—C18—C17168.8 (6)
C4—C1—N2—C2177.9 (9)N9—Rh2—N13—C19165.5 (5)
C1—N2—C2—C31.4 (10)N11—Rh2—N13—C1986 (3)
N2—C2—C3—N10.9 (10)N15—Rh2—N13—C199.7 (5)
C1—N1—C3—C20.0 (10)N19—Rh2—N13—C1977.7 (5)
Rh1—N1—C3—C2172.1 (7)Rh1—Rh2—N13—C19102.1 (5)
N7—Rh1—N3—C4170.1 (6)N9—Rh2—N13—C211.5 (9)
N5—Rh1—N3—C496 (5)N11—Rh2—N13—C2178 (3)
N1—Rh1—N3—C45.4 (6)N15—Rh2—N13—C21173.7 (9)
N17—Rh1—N3—C481.3 (6)N19—Rh2—N13—C2186.3 (8)
Rh2—Rh1—N3—C497.4 (5)Rh1—Rh2—N13—C2193.9 (8)
N7—Rh1—N3—C66.7 (9)C21—N13—C19—N141.1 (9)
N5—Rh1—N3—C681 (5)Rh2—N13—C19—N14170.3 (6)
N1—Rh1—N3—C6177.8 (9)C21—N13—C19—C22179.8 (7)
N17—Rh1—N3—C695.6 (9)Rh2—N13—C19—C2211.0 (9)
Rh2—Rh1—N3—C685.8 (8)N13—C19—N14—C200.4 (11)
C6—N3—C4—N41.4 (10)C22—C19—N14—C20178.7 (9)
Rh1—N3—C4—N4179.2 (5)C19—N14—C20—C210.5 (12)
C6—N3—C4—C1178.7 (7)N14—C20—C21—N131.2 (12)
Rh1—N3—C4—C13.5 (9)C19—N13—C21—C201.4 (10)
N1—C1—C4—N32.3 (11)Rh2—N13—C21—C20166.1 (7)
N2—C1—C4—N3178.3 (8)N13—Rh2—N15—C226.9 (5)
N1—C1—C4—N4174.2 (9)N9—Rh2—N15—C2275 (3)
N2—C1—C4—N45.3 (17)N11—Rh2—N15—C22168.6 (5)
N3—C4—N4—C51.1 (11)N19—Rh2—N15—C2280.8 (5)
C1—C4—N4—C5177.7 (9)Rh1—Rh2—N15—C2298.5 (5)
C4—N4—C5—C60.4 (12)N13—Rh2—N15—C24178.8 (8)
N4—C5—C6—N30.4 (11)N9—Rh2—N15—C2499 (3)
C4—N3—C6—C51.1 (10)N11—Rh2—N15—C245.7 (8)
Rh1—N3—C6—C5178.1 (7)N19—Rh2—N15—C2493.5 (8)
N7—Rh1—N5—C75.5 (5)Rh1—Rh2—N15—C2487.2 (8)
N3—Rh1—N5—C769 (5)C24—N15—C22—N160.5 (9)
N1—Rh1—N5—C7169.9 (5)Rh2—N15—C22—N16176.7 (5)
N17—Rh1—N5—C783.9 (5)C24—N15—C22—C19179.5 (7)
Rh2—Rh1—N5—C797.5 (5)Rh2—N15—C22—C193.2 (8)
N7—Rh1—N5—C9178.9 (8)N13—C19—C22—N155.3 (11)
N3—Rh1—N5—C9106 (5)N14—C19—C22—N15176.5 (9)
N1—Rh1—N5—C95.7 (8)N13—C19—C22—N16174.8 (8)
N17—Rh1—N5—C991.7 (8)N14—C19—C22—N163.5 (16)
Rh2—Rh1—N5—C986.9 (8)N15—C22—N16—C231.3 (10)
C9—N5—C7—N60.4 (9)C19—C22—N16—C23178.7 (9)
Rh1—N5—C7—N6176.7 (5)C22—N16—C23—C241.5 (10)
C9—N5—C7—C10179.9 (7)N16—C23—C24—N151.3 (10)
Rh1—N5—C7—C103.1 (8)C22—N15—C24—C230.5 (9)
N5—C7—N6—C81.4 (9)Rh2—N15—C24—C23174.1 (6)
C10—C7—N6—C8179.0 (8)N7—Rh1—N17—C28137.8 (7)
C7—N6—C8—C91.8 (10)N5—Rh1—N17—C2858.1 (7)
N6—C8—C9—N51.6 (10)N3—Rh1—N17—C28122.7 (7)
C7—N5—C9—C80.8 (9)N1—Rh1—N17—C2843.9 (7)
Rh1—N5—C9—C8176.5 (6)Rh2—Rh1—N17—C2834 (3)
N5—Rh1—N7—C107.5 (5)N7—Rh1—N17—C2540.6 (7)
N3—Rh1—N7—C10169.5 (5)N5—Rh1—N17—C25120.3 (7)
N1—Rh1—N7—C1099 (3)N3—Rh1—N17—C2558.9 (7)
N17—Rh1—N7—C1078.6 (5)N1—Rh1—N17—C25137.8 (7)
Rh2—Rh1—N7—C1098.1 (5)Rh2—Rh1—N17—C25145 (3)
N5—Rh1—N7—C12175.2 (9)C28—N17—C25—C260.0 (14)
N3—Rh1—N7—C121.8 (9)Rh1—N17—C25—C26178.4 (8)
N1—Rh1—N7—C1269 (4)N17—C25—C26—N180.8 (18)
N17—Rh1—N7—C1289.1 (8)C25—C26—N18—C271.0 (18)
Rh2—Rh1—N7—C1294.2 (8)C26—N18—C27—C280.4 (16)
C12—N7—C10—N82.0 (9)C25—N17—C28—C270.6 (14)
Rh1—N7—C10—N8173.7 (5)Rh1—N17—C28—C27177.9 (7)
C12—N7—C10—C7179.8 (7)N18—C27—C28—N170.4 (16)
Rh1—N7—C10—C78.1 (8)N13—Rh2—N19—C3045.7 (6)
N5—C7—C10—N73.3 (10)N9—Rh2—N19—C3054.0 (6)
N6—C7—C10—N7177.0 (8)N11—Rh2—N19—C30133.6 (6)
N5—C7—C10—N8178.9 (8)N15—Rh2—N19—C30125.5 (6)
N6—C7—C10—N80.7 (16)Rh1—Rh2—N19—C3061 (11)
N7—C10—N8—C113.1 (10)N13—Rh2—N19—C29135.4 (6)
C7—C10—N8—C11179.1 (8)N9—Rh2—N19—C29124.9 (6)
C10—N8—C11—C122.9 (10)N11—Rh2—N19—C2945.3 (6)
N8—C11—C12—N71.7 (10)N15—Rh2—N19—C2955.6 (6)
C10—N7—C12—C110.1 (10)Rh1—Rh2—N19—C29120 (11)
Rh1—N7—C12—C11168.4 (7)C30—N19—C29—C30i0.4 (12)
N13—Rh2—N9—C13169.7 (5)Rh2—N19—C29—C30i179.4 (6)
N11—Rh2—N9—C135.9 (5)C29—N19—C30—C29i0.4 (12)
N15—Rh2—N9—C1389 (3)Rh2—N19—C30—C29i179.4 (6)
N19—Rh2—N9—C1382.8 (5)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O14ii0.862.082.872 (13)154
N4—H4N···O5W0.862.082.75 (4)135
N4—H4N···O14ii0.862.553.273 (16)142
N6—H6N···O150.862.333.075 (14)145
N6—H6N···O13iii0.862.623.233 (14)129
N8—H8N···O150.862.132.915 (15)151
N8—H8N···Cl40.862.923.782 (9)178
N10—H10N···O3W0.862.002.824 (11)161
N10—H10N···O100.862.593.077 (11)117
N12—H12N···O80.862.273.062 (12)154
N12—H12N···O100.862.412.945 (11)121
N14—H14N···O11i0.862.413.001 (12)126
N14—H14N···O20.862.533.049 (14)120
N16—H16N···O4W0.862.092.910 (13)160
N16—H16N···O11i0.862.653.167 (12)120
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1/2, y+1/2, z; (iii) x, y+1, z+1.
(VIII) top
Crystal data top
C28H28F12N18Rh2·2(SiF6)·6(H2O)F(000) = 2432
Mr = 1214.78Dx = 1.887 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71069 Å
a = 27.057 (5) ÅCell parameters from 6156 reflections
b = 9.9832 (15) Åθ = 3.0–27.5°
c = 18.718 (3) ŵ = 0.95 mm1
β = 122.2560 (19)°T = 296 K
V = 4275.6 (13) Å3Prismatic, red
Z = 40.59 × 0.39 × 0.21 mm
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
4873 independent reflections
Radiation source: rotating-anode X-ray tube4409 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.025
Detector resolution: 14.62 pixels mm-1θmax = 27.5°, θmin = 3.8°
ω scansh = 3421
Absorption correction: numerical
NUMABS (Higashi, 1999)
k = 1210
Tmin = 0.747, Tmax = 0.867l = 2024
16660 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.136H atoms treated by a mixture of independent and constrained refinement
S = 1.09 w = 1/[σ2(Fo2) + (0.0767P)2 + 22.3201P]
where P = (Fo2 + 2Fc2)/3
4873 reflections(Δ/σ)max < 0.001
309 parametersΔρmax = 1.37 e Å3
0 restraintsΔρmin = 1.21 e Å3
Crystal data top
C28H28F12N18Rh2·2(SiF6)·6(H2O)V = 4275.6 (13) Å3
Mr = 1214.78Z = 4
Monoclinic, C2/cMo Kα radiation
a = 27.057 (5) ŵ = 0.95 mm1
b = 9.9832 (15) ÅT = 296 K
c = 18.718 (3) Å0.59 × 0.39 × 0.21 mm
β = 122.2560 (19)°
Data collection top
Rigaku/MSC Mercury CCD
diffractometer
4873 independent reflections
Absorption correction: numerical
NUMABS (Higashi, 1999)
4409 reflections with I > 2σ(I)
Tmin = 0.747, Tmax = 0.867Rint = 0.025
16660 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0480 restraints
wR(F2) = 0.136H atoms treated by a mixture of independent and constrained refinement
S = 1.09 w = 1/[σ2(Fo2) + (0.0767P)2 + 22.3201P]
where P = (Fo2 + 2Fc2)/3
4873 reflectionsΔρmax = 1.37 e Å3
309 parametersΔρmin = 1.21 e Å3
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 not 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
xyzUiso*/Ueq
Rh10.50000.48681 (4)0.25000.02135 (13)
Rh20.50000.21732 (4)0.25000.02278 (13)
N10.55449 (15)0.4974 (3)0.2053 (2)0.0289 (7)
C10.61052 (18)0.5151 (4)0.2656 (3)0.0316 (8)
N20.64316 (19)0.5329 (5)0.2329 (3)0.0517 (11)
H2N0.68030.54530.26060.062*
C20.6067 (3)0.5277 (8)0.1471 (4)0.0673 (18)
H20.61730.53690.10760.081*
C30.5518 (2)0.5066 (5)0.1305 (3)0.0464 (12)
H30.51810.49950.07700.056*
N30.58000 (14)0.4915 (3)0.3611 (2)0.0264 (6)
C40.62451 (18)0.5126 (4)0.3513 (3)0.0299 (8)
N40.67424 (16)0.5295 (4)0.4261 (2)0.0421 (9)
H4N0.70810.54520.43420.051*
C50.6616 (2)0.5175 (5)0.4866 (3)0.0484 (12)
H50.68790.52340.54470.058*
C60.6035 (2)0.4951 (4)0.4465 (3)0.0365 (9)
H60.58270.48390.47270.044*
N50.49934 (15)0.2108 (3)0.1393 (2)0.0292 (7)
C70.55188 (19)0.1931 (4)0.1512 (3)0.0344 (9)
N60.54808 (19)0.1764 (5)0.0777 (3)0.0460 (9)
H6N0.57690.16390.07120.055*
C80.4904 (2)0.1825 (6)0.0147 (3)0.0472 (11)
H80.47470.17430.04300.057*
C90.4605 (2)0.2030 (4)0.0536 (3)0.0369 (9)
H90.42010.21060.02630.044*
N70.58799 (14)0.2093 (3)0.2966 (2)0.0289 (7)
C100.60043 (18)0.1946 (4)0.2374 (3)0.0345 (9)
N80.65797 (17)0.1829 (5)0.2720 (3)0.0481 (10)
H8N0.67560.17330.24530.058*
C110.6838 (2)0.1889 (6)0.3576 (4)0.0525 (13)
H110.72360.18360.39800.063*
C120.64002 (19)0.2042 (4)0.3727 (3)0.0383 (9)
H120.64470.21020.42560.046*
N90.50000.7202 (4)0.25000.0237 (9)
C130.53399 (19)0.7867 (4)0.3200 (3)0.0326 (9)
H130.55800.74020.37000.039*
C140.53457 (19)0.9261 (4)0.3204 (3)0.0349 (9)
H140.55940.97180.37040.042*
N100.50000.9941 (4)0.25000.0277 (9)
Si10.81273 (6)0.5852 (2)0.41399 (10)0.0581 (4)
F10.8146 (7)0.7193 (11)0.3712 (7)0.279 (7)
F20.8735 (4)0.6493 (11)0.4859 (6)0.210 (5)
F30.8438 (4)0.5230 (10)0.3688 (7)0.214 (5)
F40.7547 (3)0.5092 (10)0.3475 (7)0.226 (6)
F50.7766 (5)0.6599 (9)0.4453 (10)0.253 (7)
F60.8270 (8)0.4585 (14)0.4673 (8)0.313 (8)
O10.5947 (3)0.8697 (6)0.1915 (4)0.0985 (18)
O20.6770 (4)0.8445 (8)0.3646 (5)0.138 (3)
O30.7085 (5)0.7199 (9)0.1683 (10)0.198 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Rh10.0230 (2)0.01753 (19)0.0232 (2)0.0000.01210 (17)0.000
Rh20.0231 (2)0.0165 (2)0.0283 (2)0.0000.01339 (17)0.000
N10.0305 (17)0.0294 (16)0.0290 (17)0.0016 (12)0.0174 (15)0.0001 (12)
C10.0285 (19)0.032 (2)0.038 (2)0.0027 (15)0.0203 (18)0.0011 (16)
N20.038 (2)0.081 (3)0.046 (2)0.013 (2)0.029 (2)0.006 (2)
C20.059 (3)0.114 (5)0.045 (3)0.023 (3)0.039 (3)0.008 (3)
C30.047 (3)0.066 (3)0.031 (2)0.011 (2)0.024 (2)0.005 (2)
N30.0275 (16)0.0229 (15)0.0263 (16)0.0010 (11)0.0127 (13)0.0002 (11)
C40.0264 (18)0.0290 (19)0.031 (2)0.0034 (14)0.0132 (16)0.0007 (14)
N40.0259 (17)0.055 (2)0.036 (2)0.0086 (16)0.0103 (16)0.0017 (17)
C50.042 (3)0.058 (3)0.031 (2)0.009 (2)0.010 (2)0.001 (2)
C60.038 (2)0.042 (2)0.028 (2)0.0036 (17)0.0166 (18)0.0011 (16)
N50.0313 (17)0.0236 (15)0.0330 (17)0.0009 (12)0.0174 (15)0.0016 (12)
C70.036 (2)0.032 (2)0.040 (2)0.0041 (17)0.0234 (19)0.0026 (17)
N60.046 (2)0.058 (2)0.044 (2)0.0068 (19)0.031 (2)0.0056 (19)
C80.051 (3)0.057 (3)0.035 (2)0.005 (2)0.024 (2)0.004 (2)
C90.038 (2)0.036 (2)0.034 (2)0.0031 (17)0.0169 (19)0.0016 (16)
N70.0267 (16)0.0215 (15)0.0377 (18)0.0013 (11)0.0166 (15)0.0002 (12)
C100.0277 (19)0.032 (2)0.045 (2)0.0039 (16)0.0201 (18)0.0016 (17)
N80.0290 (19)0.060 (2)0.057 (3)0.0052 (18)0.0243 (19)0.006 (2)
C110.027 (2)0.060 (3)0.056 (3)0.009 (2)0.013 (2)0.002 (3)
C120.030 (2)0.037 (2)0.039 (2)0.0032 (16)0.0119 (18)0.0007 (17)
N90.026 (2)0.022 (2)0.023 (2)0.0000.0129 (18)0.000
C130.040 (2)0.0222 (19)0.0237 (19)0.0040 (15)0.0086 (17)0.0028 (13)
C140.038 (2)0.0219 (19)0.031 (2)0.0025 (15)0.0092 (17)0.0006 (15)
N100.025 (2)0.027 (2)0.028 (2)0.0000.0115 (19)0.000
Si10.0305 (7)0.0998 (14)0.0438 (8)0.0039 (7)0.0197 (6)0.0054 (8)
F10.49 (2)0.151 (9)0.217 (12)0.006 (11)0.207 (14)0.057 (8)
F20.115 (6)0.308 (14)0.129 (6)0.012 (6)0.012 (5)0.095 (7)
F30.197 (8)0.295 (11)0.265 (10)0.140 (8)0.201 (8)0.178 (9)
F40.063 (4)0.219 (9)0.288 (12)0.032 (4)0.021 (5)0.121 (8)
F50.226 (10)0.194 (9)0.50 (2)0.052 (7)0.306 (13)0.127 (10)
F60.46 (2)0.270 (14)0.240 (13)0.083 (14)0.208 (15)0.175 (11)
O10.092 (4)0.099 (4)0.100 (5)0.008 (3)0.048 (4)0.008 (3)
O20.170 (8)0.126 (7)0.115 (6)0.047 (5)0.075 (6)0.036 (4)
O30.203 (10)0.126 (7)0.370 (17)0.035 (7)0.222 (12)0.012 (9)
Geometric parameters (Å, º) top
Rh1—N12.049 (3)C7—N61.334 (6)
Rh1—N1i2.049 (3)C7—C101.437 (6)
Rh1—N32.051 (3)N6—C81.366 (7)
Rh1—N3i2.051 (3)N6—H6N0.8600
Rh1—N92.330 (4)C8—C91.362 (7)
Rh1—Rh22.6904 (7)C8—H80.9300
Rh2—N7i2.054 (3)C9—H90.9300
Rh2—N72.054 (3)N7—C101.328 (6)
Rh2—N5i2.063 (3)N7—C121.368 (6)
Rh2—N52.063 (3)C10—N81.334 (6)
Rh2—N10ii2.228 (5)N8—C111.365 (7)
N1—C11.333 (6)N8—H8N0.8600
N1—C31.367 (6)C11—C121.364 (7)
C1—N21.329 (6)C11—H110.9300
C1—C41.438 (6)C12—H120.9300
N2—C21.365 (7)N9—C13i1.310 (4)
N2—H2N0.8600N9—C131.310 (4)
C2—C31.361 (8)C13—C141.391 (6)
C2—H20.9300C13—H130.9300
C3—H30.9300C14—N101.325 (5)
N3—C41.328 (5)C14—H140.9300
N3—C61.369 (5)N10—C14i1.325 (5)
C4—N41.337 (6)N10—Rh2iii2.228 (4)
N4—C51.352 (7)Si1—F61.528 (9)
N4—H4N0.8600Si1—F51.570 (6)
C5—C61.352 (7)Si1—F11.575 (9)
C5—H50.9300Si1—F41.582 (6)
C6—H60.9300Si1—F21.601 (8)
N5—C71.328 (5)Si1—F31.602 (6)
N5—C91.374 (6)
O1···O22.797 (10)O3···F4iv3.120 (14)
O1···F3iv2.895 (15)O3···F6iv3.23 (1)
O2···F52.931 (13)O3···F3iv3.254 (14)
O2···F5v3.08 (1)
N1—Rh1—N1i174.10 (18)N3—C6—H6125.3
N1—Rh1—N379.22 (14)C7—N5—C9105.8 (4)
N1i—Rh1—N3100.64 (14)C7—N5—Rh2113.7 (3)
N1—Rh1—N3i100.64 (14)C9—N5—Rh2140.0 (3)
N1i—Rh1—N3i79.22 (14)N5—C7—N6111.0 (4)
N3—Rh1—N3i177.39 (17)N5—C7—C10116.2 (4)
N1—Rh1—N987.05 (9)N6—C7—C10132.8 (4)
N1i—Rh1—N987.05 (9)C7—N6—C8108.0 (4)
N3—Rh1—N988.70 (8)C7—N6—H6N126.0
N3i—Rh1—N988.70 (8)C8—N6—H6N126.0
N1—Rh1—Rh292.95 (9)C9—C8—N6106.1 (4)
N1i—Rh1—Rh292.95 (9)C9—C8—H8127.0
N3—Rh1—Rh291.30 (8)N6—C8—H8127.0
N3i—Rh1—Rh291.30 (8)C8—C9—N5109.3 (4)
N9—Rh1—Rh2180.000 (1)C8—C9—H9125.4
N7i—Rh2—N7175.53 (17)N5—C9—H9125.4
N7i—Rh2—N5i79.18 (14)C10—N7—C12106.6 (4)
N7—Rh2—N5i100.67 (14)C10—N7—Rh2113.7 (3)
N7i—Rh2—N5100.67 (14)C12—N7—Rh2139.4 (3)
N7—Rh2—N579.18 (14)N7—C10—N8110.7 (4)
N5i—Rh2—N5176.37 (17)N7—C10—C7116.8 (4)
N7i—Rh2—N10ii87.77 (8)N8—C10—C7132.5 (4)
N7—Rh2—N10ii87.77 (8)C10—N8—C11107.5 (4)
N5i—Rh2—N10ii88.18 (9)C10—N8—H8N126.3
N5—Rh2—N10ii88.19 (9)C11—N8—H8N126.3
N7i—Rh2—Rh192.23 (8)C12—C11—N8106.9 (4)
N7—Rh2—Rh192.23 (8)C12—C11—H11126.6
N5i—Rh2—Rh191.81 (9)N8—C11—H11126.6
N5—Rh2—Rh191.81 (9)C11—C12—N7108.3 (4)
N10ii—Rh2—Rh1180.0C11—C12—H12125.9
C1—N1—C3105.8 (4)N7—C12—H12125.9
C1—N1—Rh1113.7 (3)C13i—N9—C13119.1 (4)
C3—N1—Rh1140.0 (3)C13i—N9—Rh1120.5 (2)
N2—C1—N1111.3 (4)C13—N9—Rh1120.5 (2)
N2—C1—C4132.3 (4)N9—C13—C14120.8 (4)
N1—C1—C4116.5 (4)N9—C13—H13119.6
C1—N2—C2107.3 (4)C14—C13—H13119.6
C1—N2—H2N126.4N10—C14—C13120.5 (4)
C2—N2—H2N126.4N10—C14—H14119.8
C3—C2—N2106.9 (4)C13—C14—H14119.8
C3—C2—H2126.6C14i—N10—C14118.3 (5)
N2—C2—H2126.6C14i—N10—Rh2iii120.8 (2)
C2—C3—N1108.8 (5)C14—N10—Rh2iii120.8 (2)
C2—C3—H3125.6F6—Si1—F598.0 (7)
N1—C3—H3125.6F6—Si1—F1166.1 (9)
C4—N3—C6105.5 (3)F5—Si1—F189.0 (7)
C4—N3—Rh1114.0 (3)F6—Si1—F485.2 (8)
C6—N3—Rh1140.0 (3)F5—Si1—F488.1 (5)
N3—C4—N4110.8 (4)F1—Si1—F4107.2 (7)
N3—C4—C1116.0 (4)F6—Si1—F289.6 (8)
N4—C4—C1133.2 (4)F5—Si1—F293.5 (5)
C4—N4—C5107.6 (4)F1—Si1—F277.9 (7)
C4—N4—H4N126.2F4—Si1—F2174.7 (6)
C5—N4—H4N126.2F6—Si1—F390.2 (7)
C6—C5—N4106.8 (4)F5—Si1—F3170.9 (7)
C6—C5—H5126.6F1—Si1—F383.8 (6)
N4—C5—H5126.6F4—Si1—F388.8 (5)
C5—C6—N3109.3 (4)F2—Si1—F390.3 (5)
C5—C6—H6125.3
N1—Rh1—Rh2—N7i138.71 (14)C1—C4—N4—C5179.5 (5)
N1i—Rh1—Rh2—N7i41.29 (14)C4—N4—C5—C60.9 (6)
N3—Rh1—Rh2—N7i142.02 (14)N4—C5—C6—N30.8 (6)
N3i—Rh1—Rh2—N7i37.98 (14)C4—N3—C6—C50.4 (5)
N9—Rh1—Rh2—N7i159 (100)Rh1—N3—C6—C5170.7 (3)
N1—Rh1—Rh2—N741.29 (14)N7i—Rh2—N5—C7169.9 (3)
N1i—Rh1—Rh2—N7138.71 (14)N7—Rh2—N5—C75.6 (3)
N3—Rh1—Rh2—N737.98 (14)N5i—Rh2—N5—C782.5 (3)
N3i—Rh1—Rh2—N7142.02 (14)N10ii—Rh2—N5—C782.5 (3)
N9—Rh1—Rh2—N721 (100)Rh1—Rh2—N5—C797.5 (3)
N1—Rh1—Rh2—N5i142.05 (14)N7i—Rh2—N5—C90.2 (4)
N1i—Rh1—Rh2—N5i37.95 (14)N7—Rh2—N5—C9175.2 (4)
N3—Rh1—Rh2—N5i62.78 (13)N5i—Rh2—N5—C987.1 (4)
N3i—Rh1—Rh2—N5i117.22 (13)N10ii—Rh2—N5—C987.1 (4)
N9—Rh1—Rh2—N5i122 (100)Rh1—Rh2—N5—C992.9 (4)
N1—Rh1—Rh2—N537.95 (14)C9—N5—C7—N60.7 (5)
N1i—Rh1—Rh2—N5142.05 (14)Rh2—N5—C7—N6173.8 (3)
N3—Rh1—Rh2—N5117.22 (13)C9—N5—C7—C10178.9 (4)
N3i—Rh1—Rh2—N562.78 (13)Rh2—N5—C7—C105.8 (5)
N9—Rh1—Rh2—N558 (100)N5—C7—N6—C80.4 (6)
N1—Rh1—Rh2—N10ii153 (16)C10—C7—N6—C8179.1 (5)
N1i—Rh1—Rh2—N10ii27 (16)C7—N6—C8—C90.1 (6)
N3—Rh1—Rh2—N10ii74 (16)N6—C8—C9—N50.6 (6)
N3i—Rh1—Rh2—N10ii106 (16)C7—N5—C9—C80.8 (5)
N9—Rh1—Rh2—N10ii133 (100)Rh2—N5—C9—C8170.9 (4)
N1i—Rh1—N1—C183.0 (3)N7i—Rh2—N7—C1084.1 (3)
N3—Rh1—N1—C16.3 (3)N5i—Rh2—N7—C10171.8 (3)
N3i—Rh1—N1—C1171.1 (3)N5—Rh2—N7—C104.5 (3)
N9—Rh1—N1—C183.0 (3)N10ii—Rh2—N7—C1084.1 (3)
Rh2—Rh1—N1—C197.0 (3)Rh1—Rh2—N7—C1095.9 (3)
N1i—Rh1—N1—C387.5 (5)N7i—Rh2—N7—C1289.4 (4)
N3—Rh1—N1—C3176.8 (5)N5i—Rh2—N7—C121.6 (4)
N3i—Rh1—N1—C30.6 (5)N5—Rh2—N7—C12177.9 (4)
N9—Rh1—N1—C387.5 (5)N10ii—Rh2—N7—C1289.3 (4)
Rh2—Rh1—N1—C392.5 (5)Rh1—Rh2—N7—C1290.6 (4)
C3—N1—C1—N20.9 (5)C12—N7—C10—N81.1 (5)
Rh1—N1—C1—N2174.6 (3)Rh2—N7—C10—N8176.7 (3)
C3—N1—C1—C4178.7 (4)C12—N7—C10—C7178.4 (4)
Rh1—N1—C1—C45.0 (4)Rh2—N7—C10—C72.9 (5)
N1—C1—N2—C20.6 (6)N5—C7—C10—N72.0 (6)
C4—C1—N2—C2179.0 (5)N6—C7—C10—N7177.5 (5)
C1—N2—C2—C30.0 (7)N5—C7—C10—N8178.6 (5)
N2—C2—C3—N10.6 (7)N6—C7—C10—N81.9 (9)
C1—N1—C3—C20.9 (6)N7—C10—N8—C110.6 (6)
Rh1—N1—C3—C2171.9 (4)C7—C10—N8—C11178.8 (5)
N1—Rh1—N3—C46.7 (3)C10—N8—C11—C120.1 (6)
N1i—Rh1—N3—C4167.3 (3)N8—C11—C12—N70.8 (6)
N3i—Rh1—N3—C480.6 (3)C10—N7—C12—C111.2 (5)
N9—Rh1—N3—C480.6 (3)Rh2—N7—C12—C11174.9 (4)
Rh2—Rh1—N3—C499.4 (3)N1—Rh1—N9—C13i81.1 (3)
N1—Rh1—N3—C6176.5 (4)N1i—Rh1—N9—C13i98.9 (3)
N1i—Rh1—N3—C62.5 (4)N3—Rh1—N9—C13i160.3 (3)
N3i—Rh1—N3—C689.2 (4)N3i—Rh1—N9—C13i19.7 (3)
N9—Rh1—N3—C689.2 (4)Rh2—Rh1—N9—C13i101 (100)
Rh2—Rh1—N3—C690.8 (4)N1—Rh1—N9—C1398.9 (3)
C6—N3—C4—N40.2 (5)N1i—Rh1—N9—C1381.1 (3)
Rh1—N3—C4—N4173.0 (3)N3—Rh1—N9—C1319.7 (3)
C6—N3—C4—C1179.3 (3)N3i—Rh1—N9—C13160.3 (3)
Rh1—N3—C4—C16.1 (4)Rh2—Rh1—N9—C1379 (100)
N2—C1—C4—N3179.8 (5)C13i—N9—C13—C140.5 (3)
N1—C1—C4—N30.7 (5)Rh1—N9—C13—C14179.5 (3)
N2—C1—C4—N41.4 (9)N9—C13—C14—N101.0 (6)
N1—C1—C4—N4178.1 (4)C13—C14—N10—C14i0.5 (3)
N3—C4—N4—C50.7 (5)C13—C14—N10—Rh2iii179.5 (3)
Symmetry codes: (i) x+1, y, z+1/2; (ii) x, y1, z; (iii) x, y+1, z; (iv) x+3/2, y+1/2, z+1/2; (v) x+3/2, y+3/2, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···F40.861.832.619 (9)153
N4—H4N···F50.862.092.903 (8)157
N4—H4N···F40.862.563.219 (12)135
N6—H6N···F2vi0.862.122.948 (12)161
N6—H6N···F3vi0.862.302.963 (8)134
N6—H6N···F1vi0.862.593.332 (17)145
N8—H8N···F1vi0.862.383.161 (13)152
N8—H8N···F3vi0.862.433.060 (12)131
Symmetry code: (vi) x+3/2, y1/2, z+1/2.

Experimental details

(I)(II)(III)(IV)
Crystal data
Chemical formulaC24H28N16O2Rh2·4(NO3)·4(H2O)C24H28N16O2Rh2·4(ClO4)·5(H2O)C26H32N16O2Rh2·4(ClO4)C30H38N18O2Rh2·4(BF4)
Mr1098.551266.321204.301235.84
Crystal system, space groupOrthorhombic, PbcnMonoclinic, P21/nOrthorhombic, PbcnMonoclinic, C2/c
Temperature (K)123296296296
a, b, c (Å)18.843 (3), 16.642 (3), 12.307 (2)13.453 (2), 13.334 (2), 24.906 (4)20.119 (5), 16.115 (4), 13.055 (3)16.073 (10), 19.104 (11), 16.399 (10)
α, β, γ (°)90, 90, 9090, 91.749 (2), 9090, 90, 9090, 111.673 (6), 90
V3)3859.2 (11)4465.5 (13)4232.9 (17)4679 (5)
Z4444
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.961.081.130.82
Crystal size (mm)0.66 × 0.12 × 0.100.41 × 0.35 × 0.340.42 × 0.35 × 0.320.47 × 0.38 × 0.23
Data collection
DiffractometerRigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Absorption correctionNumerical
NUMABS (Higashi, 1999)
Numerical
NUMABS (Higashi, 1999)
Numerical
NUMABS (Higashi, 1999)
Numerical
NUMABS (Higashi, 1999)
Tmin, Tmax0.809, 0.9560.731, 0.8150.740, 0.8030.765, 0.891
No. of measured, independent and
observed [I > 2σ(I)] reflections
29049, 4413, 4134 34616, 10190, 8188 30878, 4835, 4243 17721, 5356, 3475
Rint0.0420.0340.0330.056
(sin θ/λ)max1)0.6490.6490.6490.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.044, 0.080, 1.32 0.058, 0.163, 1.08 0.050, 0.126, 1.16 0.066, 0.213, 1.05
No. of reflections44161019048385356
No. of parameters313641302392
No. of restraints001474
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH-atom parameters constrained
w = 1/[σ2(Fo2) + (0.0208P)2 + 3.7755P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0753P)2 + 6.5586P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0552P)2 + 4.7874P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.1143P)2 + 8.0854P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.79, 0.570.78, 0.741.04, 0.612.60, 0.94
Absolute structure????
Absolute structure parameter????


(V)(VI)(VII)(VIII)
Crystal data
Chemical formulaC36H38N18Rh2·2(SiF6)·8(H2O)C60H60N38Rh4·SiF6·6(ClO4)·12.7(H2O)C60H60N38Rh4·8(ClO4)·11.41(H2O)C28H28F12N18Rh2·2(SiF6)·6(H2O)
Mr1356.972692.692726.261214.78
Crystal system, space groupTetragonal, I4122Orthorhombic, PbcaOrthorhombic, PbcaMonoclinic, C2/c
Temperature (K)296296296296
a, b, c (Å)17.6300 (5), 17.6300 (5), 16.8037 (6)20.170 (2), 21.875 (3), 22.541 (3)20.289 (4), 21.524 (5), 22.450 (5)27.057 (5), 9.9832 (15), 18.718 (3)
α, β, γ (°)90, 90, 9090, 90, 9090, 90, 9090, 122.2560 (19), 90
V3)5222.9 (3)9946 (2)9804 (4)4275.6 (13)
Z4444
Radiation typeMo KαMo KαMo KαMo Kα
µ (mm1)0.790.940.990.95
Crystal size (mm)0.41 × 0.40 × 0.400.50 × 0.42 × 0.310.42 × 0.35 × 0.250.59 × 0.39 × 0.21
Data collection
DiffractometerRigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Rigaku/MSC Mercury CCD
diffractometer
Absorption correctionNumerical
NUMABS (Higashi, 1999)
Numerical
NUMABS (Higashi, 1999)
Numerical
NUMABS (Higashi, 1999)
Numerical
NUMABS (Higashi, 1999)
Tmin, Tmax0.727, 0.8140.832, 0.8940.807, 0.8840.747, 0.867
No. of measured, independent and
observed [I > 2σ(I)] reflections
20508, 3004, 2952 71587, 11352, 10339 72426, 11220, 8509 16660, 4873, 4409
Rint0.0240.0350.1040.025
(sin θ/λ)max1)0.6490.6490.6490.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.027, 0.073, 1.12 0.059, 0.180, 1.17 0.092, 0.231, 1.15 0.048, 0.136, 1.09
No. of reflections300411379112204873
No. of parameters220712706309
No. of restraints1512190
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinementH atoms treated by a mixture of independent and constrained refinement
w = 1/[σ2(Fo2) + (0.0493P)2 + 1.975P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0782P)2 + 29.1806P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0905P)2 + 33.6829P]
where P = (Fo2 + 2Fc2)/3
w = 1/[σ2(Fo2) + (0.0767P)2 + 22.3201P]
where P = (Fo2 + 2Fc2)/3
Δρmax, Δρmin (e Å3)0.80, 0.361.65, 1.441.49, 1.061.37, 1.21
Absolute structureFlack H D (1983), Acta Cryst. A39, 876-881???
Absolute structure parameter0.02 (3)???

Computer programs: CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001), CrystalClear, SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), Mercury (Macrae et al., 2008), Yadokari-XG 2009 (Wakita, Nemoto et al., 2009).

Selected geometric parameters (Å, º) for (I) top
Rh1—N72.047 (2)Rh1—N12.053 (2)
Rh1—N32.048 (2)Rh1—O12.299 (2)
Rh1—N52.049 (2)Rh1—Rh1i2.6771 (6)
N7—Rh1—N399.88 (10)N5—Rh1—O190.47 (9)
N7—Rh1—N579.53 (10)N1—Rh1—O186.07 (8)
N3—Rh1—N5176.24 (9)N7—Rh1—Rh1i92.48 (6)
N7—Rh1—N1174.71 (9)N3—Rh1—Rh1i92.38 (6)
N3—Rh1—N179.74 (10)N5—Rh1—Rh1i91.36 (6)
N5—Rh1—N1100.49 (10)N1—Rh1—Rh1i92.81 (6)
N7—Rh1—O188.63 (8)O1—Rh1—Rh1i178.00 (6)
N3—Rh1—O185.80 (9)
N1—Rh1—Rh1i—N5i39.77 (10)N3—Rh1—Rh1i—N7i40.03 (10)
Symmetry code: (i) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) for (I) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O20.881.992.845 (3)162.3
N4—H4N···O30.881.942.768 (4)156.5
N6—H6N···O50.881.922.799 (4)175.2
N8—H8N···O60.882.192.981 (4)148.7
N8—H8N···O80.882.523.015 (4)116.0
O1—H1A···N9ii0.83 (5)2.57 (5)3.354 (4)158 (4)
O1—H1A···O2ii0.83 (5)2.57 (4)3.171 (3)130 (4)
O1—H1A···O4ii0.83 (5)1.93 (5)2.760 (3)174 (4)
O1—H1B···O90.78 (4)1.93 (4)2.705 (4)171 (4)
O8—H8A···O1ii0.81 (6)2.00 (6)2.808 (3)174 (5)
O8—H8B···O2i0.87 (5)2.36 (5)3.017 (4)133 (4)
O9—H9A···O7iii0.90 (6)2.12 (7)2.993 (4)164 (6)
O9—H9B···O6iv0.83 (5)2.21 (6)3.038 (4)170 (5)
O9—H9B···O7iv0.83 (5)2.56 (5)3.204 (4)135 (5)
Symmetry codes: (i) x+1, y, z+3/2; (ii) x1/2, y+1/2, z+1; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y+1/2, z1/2.
Selected geometric parameters (Å, º) for (II) top
Rh1—N72.045 (4)Rh2—N132.048 (4)
Rh1—N12.049 (4)Rh2—N112.051 (4)
Rh1—N52.050 (4)Rh2—N92.057 (4)
Rh1—N32.054 (4)Rh2—N152.061 (4)
Rh1—O12.328 (3)Rh2—O22.282 (4)
Rh1—Rh22.6488 (6)
O20···O112.790 (18)O18···O22ii2.770 (8)
O22···O12.744 (6)O23···O7ii3.070 (12)
O23···O22.678 (8)O21···O15Biii3.193 (18)
O19···O7i2.916 (9)O22···O12iv3.177 (14)
O19···O8i3.146 (11)O21···O4v3.291 (13)
O19···O5i3.018 (9)O23···O5v3.173 (12)
O20···O21i3.100 (10)O23···O4v3.281 (15)
O20···O8i3.131 (12)
N7—Rh1—N1173.08 (14)N13—Rh2—N11174.14 (14)
N7—Rh1—N579.53 (15)N13—Rh2—N999.67 (16)
N1—Rh1—N5100.15 (15)N11—Rh2—N979.56 (17)
N7—Rh1—N399.95 (15)N13—Rh2—N1579.41 (16)
N1—Rh1—N379.78 (15)N11—Rh2—N15100.95 (17)
N5—Rh1—N3175.18 (13)N9—Rh2—N15176.01 (14)
N7—Rh1—O188.46 (14)N13—Rh2—O287.62 (16)
N1—Rh1—O184.62 (14)N11—Rh2—O286.54 (16)
N5—Rh1—O186.72 (12)N9—Rh2—O288.12 (16)
N3—Rh1—O188.48 (13)N15—Rh2—O287.96 (16)
N7—Rh1—Rh293.23 (10)N13—Rh2—Rh193.64 (9)
N1—Rh1—Rh293.69 (10)N11—Rh2—Rh192.20 (10)
N5—Rh1—Rh291.67 (9)N9—Rh2—Rh191.82 (10)
N3—Rh1—Rh293.14 (10)N15—Rh2—Rh192.11 (10)
O1—Rh1—Rh2177.42 (10)O2—Rh2—Rh1178.73 (13)
N5—Rh1—Rh2—N1337.33 (15)N1—Rh1—Rh2—N937.81 (15)
N3—Rh1—Rh2—N1138.13 (16)N7—Rh1—Rh2—N1537.25 (16)
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1/2, y+1/2, z1/2; (iv) x+1/2, y1/2, z+3/2; (v) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) for (II) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O190.862.052.829 (7)150.9
N4—H4N···O190.862.273.013 (7)144.5
N4—H4N···O10vi0.862.523.104 (8)126.4
N6—H6N···O30.862.273.038 (7)148.7
N6—H6N···O1vii0.862.523.128 (5)128.2
N8—H8N···O30.862.222.991 (7)149.9
N8—H8N···O80.862.583.107 (8)120.7
N10—H10N···O110.862.183.014 (13)162.5
N12—H12N···O200.861.972.819 (8)166.8
N14—H14N···O210.862.112.884 (8)150.2
N16—H16N···O210.862.182.949 (8)148.0
Symmetry codes: (vi) x+1, y, z+1; (vii) x+1, y+1, z+1.
Selected geometric parameters (Å, º) for (III) top
Rh1—N72.040 (3)Rh1—N32.055 (3)
Rh1—N52.049 (3)Rh1—O12.307 (4)
Rh1—N12.050 (3)Rh1—Rh1i2.6752 (9)
N7—Rh1—N579.61 (12)N1—Rh1—O185.49 (12)
N7—Rh1—N1174.38 (12)N3—Rh1—O189.56 (12)
N5—Rh1—N1100.22 (12)N7—Rh1—Rh1i91.67 (9)
N7—Rh1—N399.84 (12)N5—Rh1—Rh1i91.66 (8)
N5—Rh1—N3175.47 (12)N1—Rh1—Rh1i93.95 (9)
N1—Rh1—N379.88 (12)N3—Rh1—Rh1i92.85 (9)
N7—Rh1—O188.90 (12)O1—Rh1—Rh1i177.39 (8)
N5—Rh1—O185.94 (11)
N1—Rh1—Rh1i—N5i40.76 (12)N3—Rh1—Rh1i—N7i41.15 (12)
Symmetry code: (i) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) for (III) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O20.861.982.833 (5)171.6
N4—H4N···O30.862.253.053 (6)156.4
N6—H6N···O60.862.042.897 (5)177.3
N8—H8N···O70.861.962.808 (5)170.0
O1—H1···O4ii0.805 (19)2.15 (2)2.929 (4)163 (5)
Symmetry code: (ii) x1/2, y+1/2, z+1.
Selected geometric parameters (Å, º) for (IV) top
Rh1—N72.041 (5)Rh1—N12.057 (4)
Rh1—N52.042 (4)Rh1—O12.266 (5)
Rh1—N32.049 (4)Rh1—Rh1i2.6313 (18)
N7—Rh1—N579.88 (18)N3—Rh1—O188.97 (17)
N7—Rh1—N399.97 (18)N1—Rh1—O190.60 (16)
N5—Rh1—N3173.40 (17)N7—Rh1—Rh1i92.08 (13)
N7—Rh1—N1175.25 (17)N5—Rh1—Rh1i93.04 (13)
N5—Rh1—N199.96 (18)N3—Rh1—Rh1i93.55 (13)
N3—Rh1—N179.63 (18)N1—Rh1—Rh1i92.67 (13)
N7—Rh1—O184.66 (16)O1—Rh1—Rh1i176.18 (10)
N5—Rh1—O184.44 (17)
N1—Rh1—Rh1i—N3i43.72 (18)N5—Rh1—Rh1i—N7i43.72 (17)
Symmetry code: (i) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) for (IV) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···F50.861.932.786 (8)170.1
N4—H4N···F8B0.861.972.818 (15)170.7
N4—H4N···F7A0.861.982.738 (17)145.8
N6—H6N···F4B0.861.942.773 (13)162.7
N6—H6N···F4A0.862.092.927 (16)165.9
N6—H6N···F3A0.862.543.19 (2)133.6
N8—H8N···F2A0.861.972.817 (15)166.8
N8—H8N···F2B0.862.082.884 (19)154.9
N8—H8N···F3B0.862.433.169 (19)144.2
N8—H8N···F3A0.862.563.227 (15)135.7
Selected geometric parameters (Å, º) for (V) top
Rh1—N1i2.0502 (19)Rh1—N52.275 (3)
Rh1—N32.057 (2)Rh1—Rh1ii2.7052 (5)
N5—Rh1—Rh1ii180.0
N1—Rh1ii—Rh1ii—N3
Symmetry codes: (i) y, x, z; (ii) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) for (V) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···F2iii0.861.872.684 (7)158.3
N2—H2N···F40.862.062.819 (8)147.3
N2—H2N···F50.862.232.970 (10)143.6
N2—H2N···F6iii0.862.333.004 (9)135.6
N4—H4N···F1iii0.861.922.774 (7)170.8
N4—H4N···F40.862.302.999 (9)138.3
N4—H4N···O30.862.022.744 (14)141.4
Symmetry code: (iii) x+1/2, y, z+3/4.
Selected geometric parameters (Å, º) for (VI) top
Rh1—N72.053 (4)Rh2—N132.044 (4)
Rh1—N12.056 (4)Rh2—N112.047 (4)
Rh1—N32.056 (5)Rh2—N92.048 (4)
Rh1—N52.056 (4)Rh2—N152.058 (4)
Rh1—N172.238 (4)Rh2—N192.251 (4)
Rh1—Rh22.6943 (5)
N17—Rh1—Rh2177.87 (13)N19—Rh2—Rh1179.77 (10)
N5—Rh1—Rh2—N1339.35 (17)N1—Rh1—Rh2—N938.70 (18)
N3—Rh1—Rh2—N1138.46 (18)N7—Rh1—Rh2—N1539.3 (2)
Hydrogen-bond geometry (Å, º) for (VI) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···F1i0.861.992.767 (7)149.1
N4—H4N···O7W0.861.912.773 (17)176.0
N4—H4N···O5W0.862.032.73 (3)138.1
N6—H6N···F10.861.992.794 (8)156.1
N6—H6N···F20.862.343.056 (9)141.6
N8—H8N···F30.861.942.794 (11)169.6
N10—H10N···O3W0.862.022.841 (8)159.1
N12—H12N···O80.862.273.067 (9)153.9
N12—H12N···O100.862.422.965 (9)121.9
N14—H14N···O11ii0.862.443.011 (10)124.5
N14—H14N···O20.862.543.058 (13)119.4
N16—H16N···O4W0.862.042.856 (10)158.1
N16—H16N···O11ii0.862.623.131 (10)119.6
Symmetry codes: (i) x+1/2, y+3/2, z+1; (ii) x+1, y+1, z+1.
Selected geometric parameters (Å, º) for (VII) top
Rh1—N72.043 (6)Rh2—N132.049 (6)
Rh1—N52.062 (6)Rh2—N92.050 (6)
Rh1—N32.069 (6)Rh2—N112.056 (6)
Rh1—N12.071 (6)Rh2—N152.059 (6)
Rh1—N172.235 (6)Rh2—N192.248 (6)
Rh1—Rh22.6935 (8)
N17—Rh1—Rh2176.61 (17)N19—Rh2—Rh1179.23 (16)
N5—Rh1—Rh2—N1342.5 (2)N3—Rh1—Rh2—N1141.2 (3)
N1—Rh1—Rh2—N940.5 (2)N7—Rh1—Rh2—N1542.4 (2)
Hydrogen-bond geometry (Å, º) for (VII) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O14i0.862.082.872 (13)153.6
N4—H4N···O5W0.862.082.75 (4)134.5
N4—H4N···O14i0.862.553.273 (16)142.4
N6—H6N···O150.862.333.075 (14)145.3
N6—H6N···O13ii0.862.623.233 (14)129.1
N8—H8N···O150.862.132.915 (15)151.1
N8—H8N···Cl40.862.923.782 (9)177.8
N10—H10N···O3W0.862.002.824 (11)161.3
N10—H10N···O100.862.593.077 (11)116.7
N12—H12N···O80.862.273.062 (12)153.9
N12—H12N···O100.862.412.945 (11)121.3
N14—H14N···O11iii0.862.413.001 (12)126.1
N14—H14N···O20.862.533.049 (14)119.5
N16—H16N···O4W0.862.092.910 (13)160.0
N16—H16N···O11iii0.862.653.167 (12)119.9
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x, y+1, z+1; (iii) x+1, y+1, z+1.
Selected geometric parameters (Å, º) for (VIII) top
Rh1—N12.049 (3)Rh2—N72.054 (3)
Rh1—N32.051 (3)Rh2—N52.063 (3)
Rh1—N92.330 (4)Rh2—N10i2.228 (5)
Rh1—Rh22.6904 (7)
O1···O22.797 (10)O3···F4ii3.120 (14)
O1···F3ii2.895 (15)O3···F6ii3.23 (1)
O2···F52.931 (13)O3···F3ii3.254 (14)
O2···F5iii3.08 (1)
N1—Rh1—N1iv174.10 (18)N7iv—Rh2—N7175.53 (17)
N1—Rh1—N379.22 (14)N7iv—Rh2—N5iv79.18 (14)
N1iv—Rh1—N3100.64 (14)N7—Rh2—N5iv100.67 (14)
N1—Rh1—N3iv100.64 (14)N7iv—Rh2—N5100.67 (14)
N1iv—Rh1—N3iv79.22 (14)N7—Rh2—N579.18 (14)
N3—Rh1—N3iv177.39 (17)N5iv—Rh2—N5176.37 (17)
N1—Rh1—N987.05 (9)N7iv—Rh2—N10i87.77 (8)
N1iv—Rh1—N987.05 (9)N7—Rh2—N10i87.77 (8)
N3—Rh1—N988.70 (8)N5iv—Rh2—N10i88.18 (9)
N3iv—Rh1—N988.70 (8)N5—Rh2—N10i88.19 (9)
N1—Rh1—Rh292.95 (9)N7iv—Rh2—Rh192.23 (8)
N1iv—Rh1—Rh292.95 (9)N7—Rh2—Rh192.23 (8)
N3—Rh1—Rh291.30 (8)N5iv—Rh2—Rh191.81 (9)
N3iv—Rh1—Rh291.30 (8)N5—Rh2—Rh191.81 (9)
N9—Rh1—Rh2180.000 (1)N10i—Rh2—Rh1180.0
N3—Rh1—Rh2—N737.98 (14)N1—Rh1—Rh2—N537.95 (14)
Symmetry codes: (i) x, y1, z; (ii) x+3/2, y+1/2, z+1/2; (iii) x+3/2, y+3/2, z+1; (iv) x+1, y, z+1/2.
Hydrogen-bond geometry (Å, º) for (VIII) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···F40.861.832.619 (9)152.6
N4—H4N···F50.862.092.903 (8)157.2
N4—H4N···F40.862.563.219 (12)134.7
N6—H6N···F2v0.862.122.948 (12)161.3
N6—H6N···F3v0.862.302.963 (8)134.4
N6—H6N···F1v0.862.593.332 (17)145.2
N8—H8N···F1v0.862.383.161 (13)151.5
N8—H8N···F3v0.862.433.060 (12)130.8
Symmetry code: (v) x+3/2, y1/2, z+1/2.
 

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