Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803011760/ww6071sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803011760/ww6071Isup2.hkl |
CCDC reference: 217357
The title compound was synthesized by the reaction of Ru2Cl(PhNpy)4 with a small excess of AgSbF6 in methanol–dichloromethane in the dark for 12 h. The solution changed from blue to deep red. After filtration, the filtrate was evaporated under vacuum to leave a red residue which was dissolved in dichloromethane. Well shaped crystals suitable for X-ray diffraction measurement were grown by layering diethyl ether onto the solution. [Author: "_chemical_formula_sum 'C48 H46 F6 N8 O2 Ru2 Sb'" does not match the number of H atoms in the structure, i.e. (4 x 9) + 2 + 10 = H48; please check]
The positions of the H atoms were genetared geometrically (C—H bond fixed at 0.96 Å), assigned isotropic displacement parameters and allowed to ride on their respective parent C atoms before the final cycle of least-squares refinement.
Data collection: SMART (Siemens, 1994); cell refinement: SMART and SAINT (Siemens, 1996); data reduction: XPREP (Siemens, 1997); program(s) used to solve structure: SHELXL97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
Fig. 1. A view of the cation of (I) with the atomic numbering scheme. Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity. |
[Ru2(C11H9N2)4(H2O)][SbF6]·C4H10O | F(000) = 2404 |
Mr = 1206.83 | Dx = 1.667 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5202 reflections |
a = 10.1385 (1) Å | θ = 1.3–22.5° |
b = 22.5901 (5) Å | µ = 1.25 mm−1 |
c = 21.0672 (5) Å | T = 293 K |
β = 94.860 (1)° | Block, deep red |
V = 4807.67 (16) Å3 | 0.72 × 0.46 × 0.30 mm |
Z = 4 |
Siemens SMART CCD diffractometer | 8405 independent reflections |
Radiation source: fine-focus sealed tube | 5834 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.048 |
Detector resolution: 0 pixels mm-1 | θmax = 25.1°, θmin = 1.3° |
ϕ and ω scans | h = −11→11 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −26→24 |
Tmin = 0.433, Tmax = 0.687 | l = −25→14 |
15139 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.086 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.199 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.17 | w = 1/[σ2(Fo2) + (0.0478P)2 + 41.132P] where P = (Fo2 + 2Fc2)/3 |
8405 reflections | (Δ/σ)max = 0.001 |
604 parameters | Δρmax = 0.89 e Å−3 |
0 restraints | Δρmin = −0.75 e Å−3 |
[Ru2(C11H9N2)4(H2O)][SbF6]·C4H10O | V = 4807.67 (16) Å3 |
Mr = 1206.83 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.1385 (1) Å | µ = 1.25 mm−1 |
b = 22.5901 (5) Å | T = 293 K |
c = 21.0672 (5) Å | 0.72 × 0.46 × 0.30 mm |
β = 94.860 (1)° |
Siemens SMART CCD diffractometer | 8405 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 5834 reflections with I > 2σ(I) |
Tmin = 0.433, Tmax = 0.687 | Rint = 0.048 |
15139 measured reflections |
R[F2 > 2σ(F2)] = 0.086 | 0 restraints |
wR(F2) = 0.199 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.17 | w = 1/[σ2(Fo2) + (0.0478P)2 + 41.132P] where P = (Fo2 + 2Fc2)/3 |
8405 reflections | Δρmax = 0.89 e Å−3 |
604 parameters | Δρmin = −0.75 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ru1 | 0.56687 (9) | 0.03481 (4) | 0.71563 (4) | 0.0453 (2) | |
Ru2 | 0.57751 (8) | −0.05181 (3) | 0.77213 (4) | 0.0386 (2) | |
Sb | 0.91245 (12) | 0.18550 (6) | 0.52021 (6) | 0.1028 (4) | |
O1 | 0.5563 (7) | 0.1118 (3) | 0.6675 (3) | 0.0474 (17) | |
O02 | 0.9038 (17) | 0.2341 (6) | 0.9673 (7) | 0.148 (5) | |
N1 | 0.5037 (8) | 0.0771 (4) | 0.7940 (4) | 0.046 (2) | |
N2 | 0.4719 (8) | −0.0150 (3) | 0.8383 (3) | 0.0422 (19) | |
N3 | 0.7603 (8) | 0.0518 (3) | 0.7474 (4) | 0.0426 (19) | |
N4 | 0.7466 (7) | −0.0231 (3) | 0.8209 (3) | 0.0372 (18) | |
N5 | 0.3745 (9) | 0.0139 (4) | 0.6830 (4) | 0.051 (2) | |
N6 | 0.4088 (8) | −0.0803 (4) | 0.7237 (3) | 0.0417 (19) | |
N7 | 0.6359 (8) | −0.0082 (4) | 0.6396 (3) | 0.048 (2) | |
N8 | 0.6852 (8) | −0.0880 (3) | 0.7065 (4) | 0.0422 (19) | |
F1 | 0.866 (3) | 0.2540 (7) | 0.4994 (12) | 0.391 (18) | |
F2 | 0.945 (2) | 0.1071 (9) | 0.5303 (13) | 0.339 (14) | |
F3 | 0.967 (2) | 0.1745 (13) | 0.4429 (10) | 0.326 (13) | |
F4 | 1.0718 (18) | 0.1928 (11) | 0.5543 (11) | 0.321 (12) | |
F5 | 0.8498 (18) | 0.1854 (10) | 0.5942 (6) | 0.270 (10) | |
F6 | 0.7503 (15) | 0.1608 (12) | 0.4869 (8) | 0.303 (12) | |
C01 | 0.917 (3) | 0.2865 (10) | 1.0009 (14) | 0.198 (13) | |
H01A | 0.9085 | 0.3226 | 0.9798 | 0.237* | |
C02 | 0.942 (4) | 0.2849 (11) | 1.0639 (13) | 0.26 (2) | |
H02A | 0.9475 | 0.3245 | 1.0803 | 0.388* | |
H02B | 1.0245 | 0.2648 | 1.0745 | 0.388* | |
H02C | 0.8721 | 0.2641 | 1.0824 | 0.388* | |
C03 | 0.821 (3) | 0.2307 (12) | 0.9105 (10) | 0.177 (11) | |
H03A | 0.7668 | 0.2609 | 0.8934 | 0.212* | |
C04 | 0.833 (2) | 0.1736 (8) | 0.8836 (8) | 0.123 (7) | |
H04A | 0.7766 | 0.1709 | 0.8448 | 0.184* | |
H04B | 0.8074 | 0.1442 | 0.9131 | 0.184* | |
H04C | 0.9232 | 0.1670 | 0.8748 | 0.184* | |
C12 | 0.4980 (12) | 0.1373 (5) | 0.7978 (6) | 0.064 (3) | |
H12A | 0.5291 | 0.1594 | 0.7650 | 0.077* | |
C13 | 0.4490 (13) | 0.1668 (5) | 0.8474 (6) | 0.068 (3) | |
H13A | 0.4480 | 0.2080 | 0.8487 | 0.081* | |
C14 | 0.4015 (13) | 0.1341 (5) | 0.8952 (6) | 0.066 (3) | |
H14A | 0.3656 | 0.1533 | 0.9287 | 0.079* | |
C15 | 0.4059 (11) | 0.0739 (5) | 0.8943 (5) | 0.053 (3) | |
H15A | 0.3746 | 0.0521 | 0.9273 | 0.064* | |
C16 | 0.4586 (9) | 0.0452 (4) | 0.8428 (4) | 0.041 (2) | |
C21 | 0.3929 (11) | −0.0508 (4) | 0.8760 (5) | 0.047 (2) | |
C22 | 0.2578 (11) | −0.0547 (5) | 0.8587 (5) | 0.054 (3) | |
H22A | 0.2198 | −0.0318 | 0.8253 | 0.065* | |
C23 | 0.1807 (12) | −0.0923 (5) | 0.8906 (6) | 0.066 (3) | |
H23A | 0.0902 | −0.0943 | 0.8789 | 0.079* | |
C24 | 0.2341 (13) | −0.1265 (6) | 0.9390 (6) | 0.071 (4) | |
H24A | 0.1809 | −0.1521 | 0.9601 | 0.086* | |
C25 | 0.3677 (14) | −0.1229 (6) | 0.9567 (6) | 0.081 (4) | |
H25A | 0.4046 | −0.1462 | 0.9900 | 0.098* | |
C26 | 0.4475 (13) | −0.0851 (6) | 0.9255 (5) | 0.069 (3) | |
H26A | 0.5376 | −0.0828 | 0.9378 | 0.083* | |
C32 | 0.8317 (12) | 0.0926 (5) | 0.7174 (5) | 0.057 (3) | |
H32A | 0.7908 | 0.1131 | 0.6828 | 0.068* | |
C33 | 0.9601 (13) | 0.1046 (6) | 0.7359 (6) | 0.072 (4) | |
H33A | 1.0057 | 0.1332 | 0.7147 | 0.086* | |
C34 | 1.0236 (12) | 0.0736 (5) | 0.7871 (6) | 0.065 (3) | |
H34A | 1.1122 | 0.0806 | 0.8000 | 0.079* | |
C35 | 0.9532 (10) | 0.0327 (5) | 0.8179 (5) | 0.056 (3) | |
H35A | 0.9936 | 0.0127 | 0.8530 | 0.067* | |
C36 | 0.8194 (10) | 0.0200 (4) | 0.7974 (4) | 0.042 (2) | |
C41 | 0.7863 (9) | −0.0461 (4) | 0.8824 (4) | 0.038 (2) | |
C42 | 0.7983 (11) | −0.1065 (5) | 0.8918 (5) | 0.053 (3) | |
H42A | 0.7824 | −0.1320 | 0.8574 | 0.064* | |
C43 | 0.8334 (13) | −0.1295 (6) | 0.9515 (6) | 0.069 (4) | |
H43A | 0.8413 | −0.1702 | 0.9571 | 0.083* | |
C44 | 0.8566 (12) | −0.0923 (7) | 1.0026 (5) | 0.071 (4) | |
H44A | 0.8818 | −0.1075 | 1.0428 | 0.085* | |
C45 | 0.8421 (13) | −0.0326 (6) | 0.9936 (6) | 0.073 (4) | |
H45A | 0.8575 | −0.0071 | 1.0282 | 0.087* | |
C46 | 0.8054 (12) | −0.0099 (5) | 0.9347 (5) | 0.056 (3) | |
H46A | 0.7932 | 0.0307 | 0.9299 | 0.068* | |
C52 | 0.3303 (10) | −0.0424 (5) | 0.6892 (4) | 0.046 (2) | |
C53 | 0.2013 (12) | −0.0563 (6) | 0.6614 (5) | 0.066 (3) | |
H53A | 0.1697 | −0.0948 | 0.6638 | 0.079* | |
C54 | 0.1235 (12) | −0.0140 (7) | 0.6313 (6) | 0.077 (4) | |
H54A | 0.0389 | −0.0233 | 0.6136 | 0.093* | |
C55 | 0.1717 (12) | 0.0429 (6) | 0.6273 (5) | 0.068 (4) | |
H55A | 0.1200 | 0.0721 | 0.6064 | 0.082* | |
C56 | 0.2935 (11) | 0.0560 (5) | 0.6537 (5) | 0.060 (3) | |
H56A | 0.3238 | 0.0947 | 0.6519 | 0.072* | |
C61 | 0.3826 (10) | −0.1419 (5) | 0.7209 (5) | 0.050 (3) | |
C62 | 0.3671 (13) | −0.1715 (6) | 0.6626 (6) | 0.076 (4) | |
H62A | 0.3700 | −0.1508 | 0.6246 | 0.091* | |
C63 | 0.3470 (17) | −0.2331 (7) | 0.6622 (9) | 0.109 (6) | |
H63A | 0.3355 | −0.2533 | 0.6236 | 0.131* | |
C64 | 0.3445 (15) | −0.2626 (6) | 0.7169 (9) | 0.100 (6) | |
H64A | 0.3303 | −0.3033 | 0.7157 | 0.120* | |
C65 | 0.3620 (14) | −0.2352 (6) | 0.7740 (7) | 0.078 (4) | |
H65A | 0.3605 | −0.2568 | 0.8116 | 0.093* | |
C66 | 0.3822 (11) | −0.1742 (5) | 0.7760 (6) | 0.058 (3) | |
H66A | 0.3957 | −0.1551 | 0.8151 | 0.069* | |
C72 | 0.6386 (13) | 0.0186 (6) | 0.5824 (5) | 0.071 (4) | |
H72A | 0.5972 | 0.0552 | 0.5764 | 0.085* | |
C73 | 0.6996 (15) | −0.0056 (7) | 0.5331 (6) | 0.083 (4) | |
H73A | 0.7017 | 0.0144 | 0.4946 | 0.100* | |
C74 | 0.7570 (14) | −0.0598 (7) | 0.5417 (6) | 0.079 (4) | |
H74A | 0.7975 | −0.0770 | 0.5083 | 0.095* | |
C75 | 0.7568 (12) | −0.0895 (6) | 0.5981 (5) | 0.063 (3) | |
H75A | 0.7970 | −0.1263 | 0.6036 | 0.076* | |
C76 | 0.6934 (10) | −0.0624 (5) | 0.6479 (4) | 0.048 (3) | |
C81 | 0.7720 (10) | −0.1356 (5) | 0.7259 (4) | 0.046 (2) | |
C82 | 0.9079 (12) | −0.1262 (6) | 0.7313 (5) | 0.063 (3) | |
H82A | 0.9423 | −0.0905 | 0.7181 | 0.076* | |
C83 | 0.9918 (13) | −0.1702 (6) | 0.7564 (6) | 0.075 (4) | |
H83A | 1.0829 | −0.1641 | 0.7592 | 0.090* | |
C84 | 0.9436 (15) | −0.2222 (6) | 0.7769 (6) | 0.079 (4) | |
H84A | 1.0011 | −0.2512 | 0.7942 | 0.095* | |
C85 | 0.8114 (15) | −0.2316 (5) | 0.7719 (6) | 0.073 (4) | |
H85A | 0.7779 | −0.2671 | 0.7861 | 0.088* | |
C86 | 0.7255 (12) | −0.1886 (5) | 0.7459 (6) | 0.061 (3) | |
H86A | 0.6350 | −0.1960 | 0.7420 | 0.074* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.0501 (5) | 0.0453 (5) | 0.0407 (5) | 0.0049 (4) | 0.0048 (4) | 0.0099 (4) |
Ru2 | 0.0382 (5) | 0.0405 (4) | 0.0369 (4) | 0.0010 (4) | 0.0019 (3) | 0.0030 (3) |
Sb | 0.1013 (9) | 0.1135 (9) | 0.0932 (8) | 0.0261 (7) | 0.0060 (7) | 0.0350 (7) |
O1 | 0.059 (4) | 0.038 (4) | 0.046 (4) | 0.007 (3) | 0.008 (3) | 0.023 (3) |
O02 | 0.214 (16) | 0.112 (11) | 0.120 (11) | −0.014 (11) | 0.020 (11) | −0.001 (9) |
N1 | 0.040 (5) | 0.044 (5) | 0.055 (5) | 0.010 (4) | 0.007 (4) | 0.013 (4) |
N2 | 0.052 (5) | 0.038 (4) | 0.037 (4) | −0.001 (4) | 0.007 (4) | 0.005 (3) |
N3 | 0.046 (5) | 0.037 (4) | 0.045 (4) | 0.001 (4) | 0.009 (4) | 0.010 (4) |
N4 | 0.027 (4) | 0.045 (5) | 0.040 (4) | −0.001 (4) | 0.006 (3) | 0.008 (4) |
N5 | 0.052 (6) | 0.063 (6) | 0.036 (4) | 0.011 (5) | −0.003 (4) | 0.009 (4) |
N6 | 0.037 (5) | 0.052 (5) | 0.035 (4) | −0.002 (4) | 0.000 (4) | 0.014 (4) |
N7 | 0.051 (5) | 0.059 (5) | 0.031 (4) | 0.011 (4) | −0.003 (4) | 0.004 (4) |
N8 | 0.041 (5) | 0.042 (5) | 0.042 (5) | −0.006 (4) | −0.002 (4) | −0.003 (4) |
F1 | 0.68 (5) | 0.130 (13) | 0.39 (3) | 0.17 (2) | 0.24 (3) | 0.122 (16) |
F2 | 0.33 (3) | 0.200 (18) | 0.46 (4) | 0.054 (18) | −0.14 (3) | 0.00 (2) |
F3 | 0.25 (2) | 0.51 (4) | 0.226 (19) | 0.11 (2) | 0.105 (16) | −0.01 (2) |
F4 | 0.167 (15) | 0.43 (3) | 0.36 (3) | −0.104 (18) | −0.038 (17) | −0.09 (2) |
F5 | 0.28 (2) | 0.44 (3) | 0.097 (9) | −0.013 (19) | 0.054 (11) | 0.062 (13) |
F6 | 0.148 (13) | 0.58 (4) | 0.172 (14) | 0.053 (19) | −0.054 (11) | 0.027 (19) |
C01 | 0.34 (4) | 0.083 (15) | 0.16 (2) | −0.01 (2) | −0.02 (3) | 0.015 (16) |
C02 | 0.47 (6) | 0.14 (2) | 0.15 (2) | −0.03 (3) | −0.09 (3) | −0.033 (19) |
C03 | 0.27 (3) | 0.17 (2) | 0.084 (14) | 0.03 (2) | −0.037 (17) | 0.029 (15) |
C04 | 0.169 (19) | 0.111 (14) | 0.085 (12) | 0.005 (13) | −0.005 (12) | −0.026 (11) |
C12 | 0.079 (9) | 0.045 (7) | 0.068 (8) | 0.006 (6) | 0.006 (7) | 0.011 (6) |
C13 | 0.082 (9) | 0.042 (6) | 0.079 (9) | 0.013 (6) | 0.007 (7) | −0.007 (6) |
C14 | 0.077 (9) | 0.066 (8) | 0.056 (7) | 0.013 (7) | 0.012 (6) | −0.008 (6) |
C15 | 0.059 (7) | 0.051 (7) | 0.051 (6) | −0.003 (6) | 0.011 (5) | −0.006 (5) |
C16 | 0.037 (5) | 0.042 (6) | 0.043 (5) | 0.000 (5) | −0.006 (4) | 0.002 (4) |
C21 | 0.055 (7) | 0.046 (6) | 0.042 (5) | −0.004 (5) | 0.008 (5) | −0.002 (5) |
C22 | 0.056 (7) | 0.051 (6) | 0.056 (6) | −0.001 (6) | 0.007 (5) | 0.003 (5) |
C23 | 0.054 (7) | 0.073 (8) | 0.073 (8) | −0.017 (7) | 0.017 (6) | −0.004 (7) |
C24 | 0.074 (9) | 0.073 (9) | 0.070 (8) | −0.027 (7) | 0.018 (7) | −0.003 (7) |
C25 | 0.081 (10) | 0.104 (11) | 0.058 (8) | −0.013 (8) | 0.000 (7) | 0.037 (7) |
C26 | 0.068 (8) | 0.089 (9) | 0.047 (7) | −0.013 (7) | −0.006 (6) | 0.024 (6) |
C32 | 0.069 (8) | 0.055 (7) | 0.047 (6) | −0.003 (6) | 0.008 (6) | 0.007 (5) |
C33 | 0.069 (9) | 0.074 (9) | 0.074 (9) | −0.016 (7) | 0.011 (7) | −0.010 (7) |
C34 | 0.056 (8) | 0.070 (8) | 0.071 (8) | −0.019 (6) | 0.014 (6) | 0.002 (7) |
C35 | 0.045 (7) | 0.067 (7) | 0.056 (7) | −0.011 (6) | 0.004 (5) | 0.007 (6) |
C36 | 0.050 (6) | 0.035 (5) | 0.042 (5) | 0.000 (5) | 0.005 (5) | −0.001 (4) |
C41 | 0.026 (5) | 0.046 (6) | 0.040 (5) | 0.001 (4) | −0.002 (4) | 0.002 (4) |
C42 | 0.066 (7) | 0.044 (6) | 0.050 (6) | −0.002 (5) | 0.010 (5) | 0.006 (5) |
C43 | 0.088 (10) | 0.059 (7) | 0.064 (8) | 0.011 (7) | 0.021 (7) | 0.027 (6) |
C44 | 0.067 (8) | 0.104 (11) | 0.041 (7) | 0.010 (8) | −0.001 (6) | 0.020 (7) |
C45 | 0.077 (9) | 0.094 (10) | 0.046 (7) | −0.014 (8) | −0.002 (6) | −0.012 (7) |
C46 | 0.074 (8) | 0.051 (6) | 0.043 (6) | −0.006 (6) | 0.004 (6) | 0.000 (5) |
C52 | 0.042 (6) | 0.060 (7) | 0.035 (5) | 0.000 (5) | 0.003 (4) | 0.001 (5) |
C53 | 0.057 (7) | 0.082 (9) | 0.057 (7) | 0.006 (7) | −0.008 (6) | 0.003 (6) |
C54 | 0.040 (7) | 0.128 (13) | 0.061 (8) | 0.004 (8) | −0.005 (6) | 0.027 (8) |
C55 | 0.050 (7) | 0.094 (10) | 0.059 (7) | 0.021 (7) | 0.007 (6) | 0.026 (7) |
C56 | 0.052 (7) | 0.074 (8) | 0.054 (7) | 0.008 (6) | 0.006 (5) | 0.025 (6) |
C61 | 0.045 (6) | 0.045 (6) | 0.059 (7) | −0.007 (5) | 0.002 (5) | −0.003 (5) |
C62 | 0.082 (9) | 0.074 (9) | 0.067 (8) | 0.015 (7) | −0.023 (7) | −0.024 (7) |
C63 | 0.128 (15) | 0.064 (9) | 0.125 (14) | 0.017 (10) | −0.058 (12) | −0.038 (10) |
C64 | 0.090 (11) | 0.053 (8) | 0.147 (16) | −0.001 (8) | −0.046 (11) | −0.002 (10) |
C65 | 0.083 (10) | 0.059 (8) | 0.088 (10) | 0.010 (7) | −0.015 (8) | 0.016 (7) |
C66 | 0.058 (7) | 0.046 (6) | 0.069 (8) | 0.001 (5) | 0.002 (6) | 0.000 (6) |
C72 | 0.078 (9) | 0.083 (9) | 0.051 (7) | 0.001 (7) | 0.006 (6) | 0.019 (6) |
C73 | 0.107 (12) | 0.102 (11) | 0.041 (7) | 0.018 (9) | 0.012 (7) | 0.009 (7) |
C74 | 0.095 (11) | 0.100 (11) | 0.046 (7) | 0.008 (9) | 0.021 (7) | −0.004 (7) |
C75 | 0.062 (8) | 0.079 (8) | 0.048 (7) | 0.004 (7) | 0.000 (6) | −0.004 (6) |
C76 | 0.050 (6) | 0.061 (7) | 0.033 (5) | 0.002 (5) | 0.005 (5) | 0.002 (5) |
C81 | 0.049 (6) | 0.055 (6) | 0.035 (5) | 0.004 (5) | 0.007 (5) | −0.016 (5) |
C82 | 0.054 (7) | 0.076 (8) | 0.058 (7) | 0.016 (7) | 0.002 (6) | −0.006 (6) |
C83 | 0.052 (8) | 0.090 (10) | 0.081 (9) | 0.014 (8) | −0.001 (7) | −0.029 (8) |
C84 | 0.085 (11) | 0.062 (8) | 0.086 (10) | 0.028 (8) | −0.021 (8) | −0.017 (7) |
C85 | 0.095 (11) | 0.045 (7) | 0.078 (9) | 0.006 (7) | −0.008 (8) | 0.006 (6) |
C86 | 0.058 (8) | 0.056 (7) | 0.070 (8) | −0.002 (6) | 0.004 (6) | −0.011 (6) |
Ru1—O1 | 2.012 (6) | C25—C26 | 1.382 (16) |
Ru1—N7 | 2.048 (8) | C25—H25A | 0.9300 |
Ru1—N3 | 2.054 (8) | C26—H26A | 0.9300 |
Ru1—N1 | 2.056 (8) | C32—C33 | 1.354 (16) |
Ru1—N5 | 2.067 (9) | C32—H32A | 0.9300 |
Ru1—Ru2 | 2.2882 (11) | C33—C34 | 1.397 (17) |
Ru2—N8 | 2.007 (8) | C33—H33A | 0.9300 |
Ru2—N2 | 2.008 (8) | C34—C35 | 1.365 (15) |
Ru2—N6 | 2.022 (8) | C34—H34A | 0.9300 |
Ru2—N4 | 2.029 (7) | C35—C36 | 1.417 (14) |
Sb—F1 | 1.666 (14) | C35—H35A | 0.9300 |
Sb—F4 | 1.719 (17) | C41—C46 | 1.373 (13) |
Sb—F5 | 1.732 (13) | C41—C42 | 1.382 (13) |
Sb—F3 | 1.781 (18) | C42—C43 | 1.379 (14) |
Sb—F2 | 1.810 (19) | C42—H42A | 0.9300 |
Sb—F6 | 1.820 (17) | C43—C44 | 1.369 (17) |
O02—C01 | 1.38 (3) | C43—H43A | 0.9300 |
O02—C03 | 1.40 (2) | C44—C45 | 1.369 (17) |
N1—C12 | 1.364 (13) | C44—H44A | 0.9300 |
N1—C16 | 1.368 (12) | C45—C46 | 1.366 (15) |
N2—C16 | 1.371 (12) | C45—H45A | 0.9300 |
N2—C21 | 1.426 (12) | C46—H46A | 0.9300 |
N3—C32 | 1.361 (13) | C52—C53 | 1.422 (15) |
N3—C36 | 1.370 (12) | C53—C54 | 1.362 (16) |
N4—C36 | 1.343 (12) | C53—H53A | 0.9300 |
N4—C41 | 1.421 (11) | C54—C55 | 1.379 (18) |
N5—C52 | 1.357 (13) | C54—H54A | 0.9300 |
N5—C56 | 1.369 (13) | C55—C56 | 1.343 (16) |
N6—C52 | 1.341 (12) | C55—H55A | 0.9300 |
N6—C61 | 1.417 (12) | C56—H56A | 0.9300 |
N7—C72 | 1.351 (13) | C61—C66 | 1.370 (15) |
N7—C76 | 1.359 (13) | C61—C62 | 1.395 (15) |
N8—C76 | 1.371 (12) | C62—C63 | 1.406 (19) |
N8—C81 | 1.428 (12) | C62—H62A | 0.9300 |
C01—C02 | 1.33 (3) | C63—C64 | 1.33 (2) |
C01—H01A | 0.9300 | C63—H63A | 0.9300 |
C02—H02A | 0.9600 | C64—C65 | 1.35 (2) |
C02—H02B | 0.9600 | C64—H64A | 0.9300 |
C02—H02C | 0.9600 | C65—C66 | 1.394 (16) |
C03—C04 | 1.42 (3) | C65—H65A | 0.9300 |
C03—H03A | 0.9300 | C66—H66A | 0.9300 |
C04—H04A | 0.9600 | C72—C73 | 1.368 (17) |
C04—H04B | 0.9600 | C72—H72A | 0.9300 |
C04—H04C | 0.9600 | C73—C74 | 1.361 (18) |
C12—C13 | 1.368 (16) | C73—H73A | 0.9300 |
C12—H12A | 0.9300 | C74—C75 | 1.364 (16) |
C13—C14 | 1.368 (16) | C74—H74A | 0.9300 |
C13—H13A | 0.9300 | C75—C76 | 1.416 (14) |
C14—C15 | 1.360 (15) | C75—H75A | 0.9300 |
C14—H14A | 0.9300 | C81—C86 | 1.368 (15) |
C15—C16 | 1.408 (14) | C81—C82 | 1.389 (15) |
C15—H15A | 0.9300 | C82—C83 | 1.385 (16) |
C21—C26 | 1.376 (14) | C82—H82A | 0.9300 |
C21—C22 | 1.390 (14) | C83—C84 | 1.357 (19) |
C22—C23 | 1.369 (15) | C83—H83A | 0.9300 |
C22—H22A | 0.9300 | C84—C85 | 1.352 (18) |
C23—C24 | 1.356 (17) | C84—H84A | 0.9300 |
C23—H23A | 0.9300 | C85—C86 | 1.385 (16) |
C24—C25 | 1.377 (17) | C85—H85A | 0.9300 |
C24—H24A | 0.9300 | C86—H86A | 0.9300 |
O1—Ru1—N7 | 91.3 (3) | C23—C24—H24A | 120.3 |
O1—Ru1—N3 | 90.6 (3) | C25—C24—H24A | 120.3 |
N7—Ru1—N3 | 87.9 (3) | C24—C25—C26 | 120.6 (12) |
O1—Ru1—N1 | 89.8 (3) | C24—C25—H25A | 119.7 |
N7—Ru1—N1 | 177.9 (3) | C26—C25—H25A | 119.7 |
N3—Ru1—N1 | 90.3 (3) | C21—C26—C25 | 119.7 (12) |
O1—Ru1—N5 | 91.3 (3) | C21—C26—H26A | 120.2 |
N7—Ru1—N5 | 90.4 (3) | C25—C26—H26A | 120.2 |
N3—Ru1—N5 | 177.5 (3) | C33—C32—N3 | 122.5 (11) |
N1—Ru1—N5 | 91.4 (3) | C33—C32—H32A | 118.8 |
O1—Ru1—Ru2 | 178.9 (2) | N3—C32—H32A | 118.8 |
N7—Ru1—Ru2 | 89.8 (2) | C32—C33—C34 | 119.4 (12) |
N3—Ru1—Ru2 | 89.4 (2) | C32—C33—H33A | 120.3 |
N1—Ru1—Ru2 | 89.1 (2) | C34—C33—H33A | 120.3 |
N5—Ru1—Ru2 | 88.8 (2) | C35—C34—C33 | 118.8 (12) |
N8—Ru2—N2 | 179.2 (3) | C35—C34—H34A | 120.6 |
N8—Ru2—N6 | 90.5 (3) | C33—C34—H34A | 120.6 |
N2—Ru2—N6 | 90.3 (3) | C34—C35—C36 | 121.1 (11) |
N8—Ru2—N4 | 89.6 (3) | C34—C35—H35A | 119.4 |
N2—Ru2—N4 | 89.6 (3) | C36—C35—H35A | 119.4 |
N6—Ru2—N4 | 179.9 (4) | N4—C36—N3 | 116.5 (9) |
N8—Ru2—Ru1 | 89.6 (2) | N4—C36—C35 | 125.1 (9) |
N2—Ru2—Ru1 | 90.2 (2) | N3—C36—C35 | 118.3 (9) |
N6—Ru2—Ru1 | 90.5 (2) | C46—C41—C42 | 117.9 (9) |
N4—Ru2—Ru1 | 89.5 (2) | C46—C41—N4 | 121.5 (9) |
F1—Sb—F4 | 104.8 (14) | C42—C41—N4 | 120.4 (9) |
F1—Sb—F5 | 97.0 (10) | C43—C42—C41 | 121.0 (11) |
F4—Sb—F5 | 91.6 (10) | C43—C42—H42A | 119.5 |
F1—Sb—F3 | 89.5 (11) | C41—C42—H42A | 119.5 |
F4—Sb—F3 | 92.4 (11) | C44—C43—C42 | 120.0 (11) |
F5—Sb—F3 | 171.3 (12) | C44—C43—H43A | 120.0 |
F1—Sb—F2 | 169.8 (13) | C42—C43—H43A | 120.0 |
F4—Sb—F2 | 83.8 (11) | C45—C44—C43 | 119.2 (11) |
F5—Sb—F2 | 88.2 (12) | C45—C44—H44A | 120.4 |
F3—Sb—F2 | 84.5 (12) | C43—C44—H44A | 120.4 |
F1—Sb—F6 | 87.6 (13) | C46—C45—C44 | 120.8 (11) |
F4—Sb—F6 | 167.6 (12) | C46—C45—H45A | 119.6 |
F5—Sb—F6 | 87.6 (8) | C44—C45—H45A | 119.6 |
F3—Sb—F6 | 86.9 (10) | C45—C46—C41 | 121.0 (11) |
F2—Sb—F6 | 83.8 (11) | C45—C46—H46A | 119.5 |
C01—O02—C03 | 121 (2) | C41—C46—H46A | 119.5 |
C12—N1—C16 | 117.6 (9) | N6—C52—N5 | 117.7 (9) |
C12—N1—Ru1 | 121.9 (7) | N6—C52—C53 | 124.4 (10) |
C16—N1—Ru1 | 120.4 (7) | N5—C52—C53 | 117.8 (10) |
C16—N2—C21 | 117.4 (8) | C54—C53—C52 | 120.9 (13) |
C16—N2—Ru2 | 121.4 (6) | C54—C53—H53A | 119.6 |
C21—N2—Ru2 | 120.7 (6) | C52—C53—H53A | 119.6 |
C32—N3—C36 | 119.8 (9) | C53—C54—C55 | 119.2 (12) |
C32—N3—Ru1 | 120.4 (7) | C53—C54—H54A | 120.4 |
C36—N3—Ru1 | 119.7 (6) | C55—C54—H54A | 120.4 |
C36—N4—C41 | 118.7 (8) | C56—C55—C54 | 119.8 (11) |
C36—N4—Ru2 | 120.8 (6) | C56—C55—H55A | 120.1 |
C41—N4—Ru2 | 120.4 (6) | C54—C55—H55A | 120.1 |
C52—N5—C56 | 120.2 (10) | C55—C56—N5 | 122.0 (12) |
C52—N5—Ru1 | 119.5 (7) | C55—C56—H56A | 119.0 |
C56—N5—Ru1 | 120.3 (8) | N5—C56—H56A | 119.0 |
C52—N6—C61 | 120.3 (8) | C66—C61—C62 | 118.8 (11) |
C52—N6—Ru2 | 120.5 (7) | C66—C61—N6 | 120.1 (9) |
C61—N6—Ru2 | 118.8 (6) | C62—C61—N6 | 120.9 (10) |
C72—N7—C76 | 118.6 (9) | C61—C62—C63 | 119.0 (14) |
C72—N7—Ru1 | 121.2 (8) | C61—C62—H62A | 120.5 |
C76—N7—Ru1 | 119.8 (6) | C63—C62—H62A | 120.5 |
C76—N8—C81 | 119.6 (8) | C64—C63—C62 | 120.2 (14) |
C76—N8—Ru2 | 121.8 (7) | C64—C63—H63A | 119.9 |
C81—N8—Ru2 | 117.8 (6) | C62—C63—H63A | 119.9 |
C02—C01—O02 | 119 (2) | C63—C64—C65 | 122.0 (14) |
C02—C01—H01A | 120.3 | C63—C64—H64A | 119.0 |
O02—C01—H01A | 120.3 | C65—C64—H64A | 119.0 |
C01—C02—H02A | 109.5 | C64—C65—C66 | 119.1 (13) |
C01—C02—H02B | 109.5 | C64—C65—H65A | 120.4 |
H02A—C02—H02B | 109.5 | C66—C65—H65A | 120.4 |
C01—C02—H02C | 109.5 | C61—C66—C65 | 120.8 (12) |
H02A—C02—H02C | 109.5 | C61—C66—H66A | 119.6 |
H02B—C02—H02C | 109.5 | C65—C66—H66A | 119.6 |
O02—C03—C04 | 109.0 (19) | N7—C72—C73 | 122.8 (12) |
O02—C03—H03A | 125.5 | N7—C72—H72A | 118.6 |
C04—C03—H03A | 125.5 | C73—C72—H72A | 118.6 |
C03—C04—H04A | 109.5 | C74—C73—C72 | 118.3 (12) |
C03—C04—H04B | 109.5 | C74—C73—H73A | 120.8 |
H04A—C04—H04B | 109.5 | C72—C73—H73A | 120.8 |
C03—C04—H04C | 109.5 | C73—C74—C75 | 121.7 (12) |
H04A—C04—H04C | 109.5 | C73—C74—H74A | 119.1 |
H04B—C04—H04C | 109.5 | C75—C74—H74A | 119.1 |
N1—C12—C13 | 123.5 (11) | C74—C75—C76 | 117.9 (12) |
N1—C12—H12A | 118.3 | C74—C75—H75A | 121.1 |
C13—C12—H12A | 118.3 | C76—C75—H75A | 121.1 |
C12—C13—C14 | 118.1 (11) | N7—C76—N8 | 116.0 (9) |
C12—C13—H13A | 120.9 | N7—C76—C75 | 120.6 (9) |
C14—C13—H13A | 120.9 | N8—C76—C75 | 123.4 (10) |
C15—C14—C13 | 121.1 (11) | C86—C81—C82 | 118.3 (11) |
C15—C14—H14A | 119.5 | C86—C81—N8 | 121.9 (10) |
C13—C14—H14A | 119.5 | C82—C81—N8 | 119.4 (10) |
C14—C15—C16 | 119.1 (11) | C83—C82—C81 | 119.6 (12) |
C14—C15—H15A | 120.4 | C83—C82—H82A | 120.2 |
C16—C15—H15A | 120.4 | C81—C82—H82A | 120.2 |
N1—C16—N2 | 115.4 (9) | C84—C83—C82 | 121.2 (13) |
N1—C16—C15 | 120.6 (9) | C84—C83—H83A | 119.4 |
N2—C16—C15 | 123.9 (9) | C82—C83—H83A | 119.4 |
C26—C21—C22 | 119.2 (10) | C85—C84—C83 | 119.5 (12) |
C26—C21—N2 | 122.1 (10) | C85—C84—H84A | 120.3 |
C22—C21—N2 | 118.5 (9) | C83—C84—H84A | 120.3 |
C23—C22—C21 | 120.1 (11) | C84—C85—C86 | 120.4 (13) |
C23—C22—H22A | 119.9 | C84—C85—H85A | 119.8 |
C21—C22—H22A | 119.9 | C86—C85—H85A | 119.8 |
C24—C23—C22 | 121.0 (12) | C81—C86—C85 | 121.0 (12) |
C24—C23—H23A | 119.5 | C81—C86—H86A | 119.5 |
C22—C23—H23A | 119.5 | C85—C86—H86A | 119.5 |
C23—C24—C25 | 119.5 (12) |
Experimental details
Crystal data | |
Chemical formula | [Ru2(C11H9N2)4(H2O)][SbF6]·C4H10O |
Mr | 1206.83 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 10.1385 (1), 22.5901 (5), 21.0672 (5) |
β (°) | 94.860 (1) |
V (Å3) | 4807.67 (16) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.25 |
Crystal size (mm) | 0.72 × 0.46 × 0.30 |
Data collection | |
Diffractometer | Siemens SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.433, 0.687 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 15139, 8405, 5834 |
Rint | 0.048 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.086, 0.199, 1.17 |
No. of reflections | 8405 |
No. of parameters | 604 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
w = 1/[σ2(Fo2) + (0.0478P)2 + 41.132P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 0.89, −0.75 |
Computer programs: SMART (Siemens, 1994), SMART and SAINT (Siemens, 1996), XPREP (Siemens, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.
Ru1—O1 | 2.012 (6) | Sb—F4 | 1.719 (17) |
Ru1—N7 | 2.048 (8) | Sb—F3 | 1.781 (18) |
Ru1—N3 | 2.054 (8) | Sb—F6 | 1.820 (17) |
Ru1—N1 | 2.056 (8) | C44—C45 | 1.369 (17) |
Ru1—N5 | 2.067 (9) | C45—C46 | 1.366 (15) |
Ru1—Ru2 | 2.2882 (11) | C52—C53 | 1.422 (15) |
Ru2—N8 | 2.007 (8) | C83—C84 | 1.357 (19) |
Ru2—N6 | 2.022 (8) | C85—C86 | 1.385 (16) |
O1—Ru1—N7 | 91.3 (3) | C76—N8—C81 | 119.6 (8) |
N7—Ru1—N3 | 87.9 (3) | H02A—C02—H02B | 109.5 |
N3—Ru1—N1 | 90.3 (3) | O02—C03—C04 | 109.0 (19) |
N1—Ru1—N5 | 91.4 (3) | N1—C12—C13 | 123.5 (11) |
N7—Ru1—Ru2 | 89.8 (2) | C14—C15—C16 | 119.1 (11) |
N8—Ru2—N2 | 179.2 (3) | C23—C22—C21 | 120.1 (11) |
N2—Ru2—N4 | 89.6 (3) | C43—C42—C41 | 121.0 (11) |
N4—Ru2—Ru1 | 89.5 (2) | C46—C45—C44 | 120.8 (11) |
F4—Sb—F5 | 91.6 (10) | C54—C53—C52 | 120.9 (13) |
F4—Sb—F2 | 83.8 (11) | C64—C63—C62 | 120.2 (14) |
F4—Sb—F6 | 167.6 (12) | C74—C75—C76 | 117.9 (12) |
C12—N1—Ru1 | 121.9 (7) | C83—C82—C81 | 119.6 (12) |
C36—N4—Ru2 | 120.8 (6) | C84—C85—C86 | 120.4 (13) |
C52—N6—Ru2 | 120.5 (7) |
In the chemistry of multiple-bonded diruthenium complexes, a variety of diruthenium compounds have been reported (Cotton & Walton, 1985; Tooze et al., 1984; Chakravarty & Cotton, 1975) many years ago. In most cases, spectral and electrochemical studies on the diruthenium complexes show that modification of the axial ligand usually results in dramatic shift of the visible band energy and the redox potentials. These complexes of RuII–RuIII are quite different from those of other dimetallic species. The cationic species [Ru2(µ2-PhNpy)4·H2O]+ consists of a diruthenium core held by four PhNpy ligands. The ruthenium(III) that is bonded to pyridine N atoms has an axial H2O while the axial site on the other ruthenium(II) is vacant. The molecular structure of Ru2Cl(PhNpy)4 has already been reported (Chakravarty et al., 1985). The two molecules are very similar in structure except that the Ru—Cl bond in Ru2Cl(PhNpy)4 is replaced by Ru—OH2. This change has a little effect on the Ru—Ru distance, which changes from 2.275 (3) Å in Ru2Cl(PhNpy)4 to 2.288 (1) Å in [Ru2(ap)4(H2O)](SbF6). The average RuII—N distance is 2.014 (6) Å but RuIII—N is 2.056 (8) Å in the title compound, with the O1—Ru1—Ru2 angle being 178.80 (18)°