Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803006573/tk6099sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803006573/tk6099Isup2.hkl |
CCDC reference: 209906
The title compound was prepared from the reaction of [RuCl2(PPh3)3] and S[Si(CH3)3]2 in refluxing tetrahydrofuran for 16 h. After this time, the reaction was cooled to room temperature and filtered and the solvent volume reduced in vacuo (ca 5 ml). Microcrystals suitable for single-crystal X-ray diffraction analysis were grown from the reaction solution at 243 K.
The asymmetric unit contains the complex cluster molecule (I) and four partially occupied tetrahydrofuran solvate sites. Additionally, there are four sites treated as partially occupied water O-atom sites, although they may be associated with further disordered and unresolved tetrahydrofuran sites. In general, the non-H-atom sites were modelled with anisotropic displacement parameters, and a riding atom model was used for the H atoms. The partially occupied non-H sites were modelled with isotropic displacement parameters. No H atoms were included in the model for the water sites.
Data collection: SMART–KAPPA (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT and XPREP (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: TEXSAN for Windows (Molecular Structure Corporation, 1997), Xtal3.6 (Hall et al., 1999), ORTEPII (Johnson, 1976) and WinGX (Farrugia, 1999).
Fig. 1. ORTEPII (Johnson, 1976; Hall et al., 1999) projection of (I), with displacement ellipsoids shown at the 20% probability level. |
[Ru3Cl4S(C18H15P)6]·1.25C4H8O·0.75H2O | Z = 2 |
Mr = 2152.82 | F(000) = 2200 |
Triclinic, P1 | Dx = 1.365 Mg m−3 |
a = 14.183 (4) Å | Synchrotron radiation, λ = 0.55940 Å |
b = 14.699 (5) Å | Cell parameters from 1021 reflections |
c = 25.814 (9) Å | θ = 2.3–19.4° |
α = 91.904 (11)° | µ = 0.37 mm−1 |
β = 92.328 (11)° | T = 123 K |
γ = 102.784 (11)° | Prism, red |
V = 5239 (3) Å3 | 0.08 × 0.03 × 0.02 mm |
SMART 6000 detector mounted on a Bruker Kappa Platform diffractometer | 15139 independent reflections |
Radiation source: ChemMatCARS, APS, Argonne National Lab, USA | 12160 reflections with I > 2σ(I) |
Double Diamond 111 monochromator | Rint = 0.049 |
ϕ scans | θmax = 19.0°, θmin = 1.3° |
Absorption correction: multi-scan (SADABS; Blessings, 1995; Sheldrick, 1996) | h = −14→14 |
Tmin = 0.987, Tmax = 0.995 | k = −16→16 |
109758 measured reflections | l = −29→29 |
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)] = 0.089 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.243 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.42 | w = 1/[σ2(Fo2) + (0.06P)2 + 6P] where P = (Fo2 + 2Fc2)/3 |
15139 reflections | (Δ/σ)max = 0.001 |
1156 parameters | Δρmax = 1.38 e Å−3 |
30 restraints | Δρmin = −1.25 e Å−3 |
[Ru3Cl4S(C18H15P)6]·1.25C4H8O·0.75H2O | γ = 102.784 (11)° |
Mr = 2152.82 | V = 5239 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 14.183 (4) Å | Synchrotron radiation, λ = 0.55940 Å |
b = 14.699 (5) Å | µ = 0.37 mm−1 |
c = 25.814 (9) Å | T = 123 K |
α = 91.904 (11)° | 0.08 × 0.03 × 0.02 mm |
β = 92.328 (11)° |
SMART 6000 detector mounted on a Bruker Kappa Platform diffractometer | 15139 independent reflections |
Absorption correction: multi-scan (SADABS; Blessings, 1995; Sheldrick, 1996) | 12160 reflections with I > 2σ(I) |
Tmin = 0.987, Tmax = 0.995 | Rint = 0.049 |
109758 measured reflections |
R[F2 > 2σ(F2)] = 0.089 | 30 restraints |
wR(F2) = 0.243 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.42 | Δρmax = 1.38 e Å−3 |
15139 reflections | Δρmin = −1.25 e Å−3 |
1156 parameters |
Experimental. Data were collected with a 360° ϕ scan using 0.3° increments. A multi-scan empirical correction for absorption, decay and any beam inhomogeneity determined with SADABS (Sheldrick, 1996; Blessing, 1995) was applied to the data. The data integration and reduction were undertaken with SAINT and XPREP (Bruker, 2001) and subsequent computations were carried out with the TEXSAN (Molecular Structure Corporation, 1995), WinGX (Farrugia, 1999) and Xtal3.6 (Hall et al., 1999) graphical user interfaces. The data reduction included the application of Lorentz and polarization corrections. The structure was solved in the space group P1 by direct methods with SHELXS97 (Sheldrick, 1997), and extended and refined with SHELXL97 (Sheldrick, 1997). |
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 | Occ. (<1) | |
Ru1 | 0.89559 (7) | 0.62445 (6) | 0.20081 (3) | 0.0232 (2) | |
Ru2 | 0.80558 (7) | 0.39975 (6) | 0.21930 (3) | 0.0234 (2) | |
Ru3 | 0.72397 (7) | 0.56132 (6) | 0.28474 (3) | 0.0240 (2) | |
Cl1 | 0.93095 (15) | 0.48085 (14) | 0.16220 (7) | 0.0150 (4) | |
Cl2 | 0.69038 (16) | 0.39337 (15) | 0.28507 (8) | 0.0196 (5) | |
Cl3 | 0.81337 (17) | 0.71697 (14) | 0.25731 (7) | 0.0187 (5) | |
Cl4 | 0.89304 (16) | 0.53285 (14) | 0.28059 (7) | 0.0161 (4) | |
S1 | 0.73580 (16) | 0.52788 (14) | 0.19423 (7) | 0.0133 (4) | |
P1 | 1.06235 (17) | 0.69304 (15) | 0.21911 (8) | 0.0146 (5) | |
P2 | 0.87108 (17) | 0.71042 (15) | 0.13116 (8) | 0.0139 (5) | |
P3 | 0.88843 (17) | 0.29634 (15) | 0.26054 (8) | 0.0162 (5) | |
P4 | 0.72402 (17) | 0.29389 (15) | 0.15516 (8) | 0.0136 (5) | |
P5 | 0.74561 (18) | 0.60469 (17) | 0.37448 (8) | 0.0181 (5) | |
P6 | 0.56313 (17) | 0.56460 (16) | 0.27658 (8) | 0.0161 (5) | |
C1 | 1.0994 (7) | 0.8097 (6) | 0.2528 (3) | 0.021 (2) | |
C2 | 1.0460 (8) | 0.8271 (7) | 0.2949 (4) | 0.030 (2) | |
H2 | 0.9946 | 0.7796 | 0.3057 | 0.036* | |
C3 | 1.0688 (9) | 0.9161 (8) | 0.3214 (4) | 0.042 (3) | |
H3 | 1.0313 | 0.9286 | 0.3493 | 0.050* | |
C4 | 1.1444 (10) | 0.9836 (8) | 0.3069 (5) | 0.045 (3) | |
H4 | 1.1615 | 1.0416 | 0.3261 | 0.054* | |
C5 | 1.1960 (10) | 0.9684 (7) | 0.2649 (5) | 0.044 (3) | |
H5 | 1.2467 | 1.0168 | 0.2542 | 0.052* | |
C6 | 1.1739 (8) | 0.8816 (6) | 0.2378 (4) | 0.028 (2) | |
H6 | 1.2101 | 0.8714 | 0.2088 | 0.033* | |
C7 | 1.1491 (7) | 0.7020 (6) | 0.1668 (3) | 0.019 (2) | |
C8 | 1.2485 (7) | 0.7227 (7) | 0.1793 (4) | 0.025 (2) | |
H8 | 1.2709 | 0.7318 | 0.2147 | 0.031* | |
C9 | 1.3150 (8) | 0.7302 (7) | 0.1410 (4) | 0.033 (2) | |
H9 | 1.3824 | 0.7466 | 0.1501 | 0.039* | |
C10 | 1.2830 (9) | 0.7137 (8) | 0.0895 (4) | 0.039 (3) | |
H10 | 1.3286 | 0.7179 | 0.0632 | 0.047* | |
C11 | 1.1856 (8) | 0.6911 (7) | 0.0762 (3) | 0.027 (2) | |
H11 | 1.1638 | 0.6796 | 0.0408 | 0.033* | |
C12 | 1.1187 (8) | 0.6852 (6) | 0.1149 (3) | 0.023 (2) | |
H12 | 1.0514 | 0.6695 | 0.1055 | 0.028* | |
C13 | 1.1240 (7) | 0.6233 (6) | 0.2623 (3) | 0.020 (2) | |
C14 | 1.1548 (7) | 0.6505 (7) | 0.3138 (3) | 0.022 (2) | |
H14 | 1.1393 | 0.7046 | 0.3293 | 0.026* | |
C15 | 1.2077 (7) | 0.5991 (7) | 0.3423 (4) | 0.028 (2) | |
H15 | 1.2273 | 0.6176 | 0.3774 | 0.033* | |
C16 | 1.2321 (8) | 0.5214 (7) | 0.3203 (4) | 0.030 (2) | |
H16 | 1.2707 | 0.4879 | 0.3396 | 0.036* | |
C17 | 1.2000 (8) | 0.4925 (7) | 0.2697 (4) | 0.031 (2) | |
H17 | 1.2149 | 0.4376 | 0.2549 | 0.037* | |
C18 | 1.1470 (7) | 0.5419 (6) | 0.2406 (4) | 0.021 (2) | |
H18 | 1.1258 | 0.5213 | 0.2059 | 0.025* | |
C19 | 0.7548 (7) | 0.7470 (6) | 0.1282 (3) | 0.0147 (18) | |
C20 | 0.6693 (7) | 0.6779 (6) | 0.1168 (3) | 0.0177 (19) | |
H20 | 0.6718 | 0.6139 | 0.1145 | 0.021* | |
C21 | 0.5821 (7) | 0.7036 (7) | 0.1089 (3) | 0.023 (2) | |
H21 | 0.5247 | 0.6568 | 0.1016 | 0.027* | |
C22 | 0.5772 (8) | 0.7964 (7) | 0.1114 (4) | 0.029 (2) | |
H22 | 0.5172 | 0.8135 | 0.1046 | 0.035* | |
C23 | 0.6607 (9) | 0.8649 (7) | 0.1240 (5) | 0.038 (3) | |
H23 | 0.6576 | 0.9288 | 0.1264 | 0.046* | |
C24 | 0.7477 (7) | 0.8401 (6) | 0.1329 (4) | 0.026 (2) | |
H24 | 0.8039 | 0.8870 | 0.1424 | 0.032* | |
C25 | 0.9549 (7) | 0.8244 (6) | 0.1273 (3) | 0.0179 (19) | |
C26 | 0.9705 (8) | 0.8857 (6) | 0.1710 (4) | 0.025 (2) | |
H26 | 0.9396 | 0.8656 | 0.2019 | 0.030* | |
C27 | 1.0299 (8) | 0.9756 (6) | 0.1710 (4) | 0.030 (2) | |
H27 | 1.0367 | 1.0167 | 0.2008 | 0.036* | |
C28 | 1.0789 (8) | 1.0035 (7) | 0.1265 (4) | 0.034 (3) | |
H28 | 1.1215 | 1.0632 | 0.1262 | 0.041* | |
C29 | 1.0655 (8) | 0.9436 (7) | 0.0824 (4) | 0.033 (2) | |
H29 | 1.0982 | 0.9631 | 0.0520 | 0.040* | |
C30 | 1.0041 (7) | 0.8553 (6) | 0.0829 (4) | 0.023 (2) | |
H30 | 0.9956 | 0.8152 | 0.0527 | 0.028* | |
C31 | 0.8648 (7) | 0.6649 (6) | 0.0620 (3) | 0.0177 (19) | |
C32 | 0.8245 (6) | 0.7113 (6) | 0.0232 (3) | 0.0158 (18) | |
H32 | 0.8005 | 0.7649 | 0.0320 | 0.019* | |
C33 | 0.8195 (7) | 0.6789 (6) | −0.0283 (3) | 0.021 (2) | |
H33 | 0.7928 | 0.7113 | −0.0543 | 0.025* | |
C34 | 0.8526 (7) | 0.6008 (7) | −0.0423 (3) | 0.024 (2) | |
H34 | 0.8480 | 0.5789 | −0.0776 | 0.028* | |
C35 | 0.8929 (7) | 0.5543 (6) | −0.0040 (3) | 0.021 (2) | |
H35 | 0.9157 | 0.5001 | −0.0133 | 0.026* | |
C36 | 0.9000 (6) | 0.5866 (6) | 0.0477 (3) | 0.0149 (18) | |
H36 | 0.9291 | 0.5553 | 0.0734 | 0.018* | |
C37 | 1.0080 (7) | 0.2850 (6) | 0.2398 (3) | 0.0168 (18) | |
C38 | 1.0290 (7) | 0.2962 (6) | 0.1885 (3) | 0.021 (2) | |
H38 | 0.9849 | 0.3158 | 0.1650 | 0.025* | |
C39 | 1.1163 (8) | 0.2785 (7) | 0.1710 (4) | 0.029 (2) | |
H39 | 1.1307 | 0.2862 | 0.1356 | 0.035* | |
C40 | 1.1812 (8) | 0.2498 (7) | 0.2048 (4) | 0.030 (2) | |
H40 | 1.2401 | 0.2385 | 0.1927 | 0.036* | |
C41 | 1.1597 (8) | 0.2379 (7) | 0.2558 (4) | 0.033 (2) | |
H41 | 1.2035 | 0.2171 | 0.2789 | 0.040* | |
C42 | 1.0746 (8) | 0.2560 (7) | 0.2737 (4) | 0.027 (2) | |
H42 | 1.0612 | 0.2488 | 0.3093 | 0.032* | |
C43 | 0.8296 (7) | 0.1710 (6) | 0.2662 (3) | 0.021 (2) | |
C44 | 0.8805 (8) | 0.0994 (7) | 0.2634 (4) | 0.030 (2) | |
H44 | 0.9477 | 0.1151 | 0.2574 | 0.036* | |
C45 | 0.8358 (9) | 0.0062 (7) | 0.2690 (4) | 0.036 (3) | |
H45 | 0.8720 | −0.0409 | 0.2670 | 0.044* | |
C46 | 0.7382 (10) | −0.0171 (7) | 0.2776 (5) | 0.042 (3) | |
H46 | 0.7063 | −0.0803 | 0.2818 | 0.050* | |
C47 | 0.6867 (9) | 0.0543 (7) | 0.2802 (4) | 0.036 (3) | |
H47 | 0.6194 | 0.0391 | 0.2860 | 0.043* | |
C48 | 0.7328 (7) | 0.1465 (7) | 0.2745 (4) | 0.027 (2) | |
H48 | 0.6966 | 0.1936 | 0.2764 | 0.032* | |
C49 | 0.9155 (8) | 0.3285 (7) | 0.3308 (3) | 0.024 (2) | |
C50 | 1.0007 (8) | 0.3934 (7) | 0.3472 (4) | 0.028 (2) | |
H50 | 1.0425 | 0.4233 | 0.3220 | 0.034* | |
C51 | 1.0246 (9) | 0.4144 (9) | 0.3991 (4) | 0.044 (3) | |
H51 | 1.0848 | 0.4550 | 0.4095 | 0.053* | |
C52 | 0.9603 (10) | 0.3760 (10) | 0.4365 (4) | 0.049 (3) | |
H52 | 0.9761 | 0.3917 | 0.4723 | 0.058* | |
C53 | 0.8754 (10) | 0.3164 (9) | 0.4214 (4) | 0.046 (3) | |
H53 | 0.8312 | 0.2915 | 0.4467 | 0.055* | |
C54 | 0.8526 (8) | 0.2914 (8) | 0.3693 (4) | 0.033 (2) | |
H54 | 0.7935 | 0.2485 | 0.3595 | 0.039* | |
C55 | 0.8031 (7) | 0.2337 (6) | 0.1188 (3) | 0.0179 (19) | |
C56 | 0.8531 (7) | 0.2781 (6) | 0.0778 (3) | 0.0173 (18) | |
H56 | 0.8422 | 0.3363 | 0.0672 | 0.021* | |
C57 | 0.9189 (7) | 0.2369 (7) | 0.0525 (3) | 0.024 (2) | |
H57 | 0.9531 | 0.2678 | 0.0249 | 0.029* | |
C58 | 0.9354 (8) | 0.1510 (6) | 0.0669 (3) | 0.025 (2) | |
H58 | 0.9797 | 0.1229 | 0.0491 | 0.030* | |
C59 | 0.8857 (7) | 0.1075 (6) | 0.1077 (4) | 0.023 (2) | |
H59 | 0.8952 | 0.0484 | 0.1177 | 0.028* | |
C60 | 0.8225 (7) | 0.1495 (6) | 0.1342 (3) | 0.020 (2) | |
H60 | 0.7919 | 0.1204 | 0.1633 | 0.024* | |
C61 | 0.6217 (7) | 0.1973 (6) | 0.1701 (3) | 0.0188 (19) | |
C62 | 0.6008 (8) | 0.1097 (7) | 0.1437 (4) | 0.029 (2) | |
H62 | 0.6436 | 0.0962 | 0.1187 | 0.034* | |
C63 | 0.5171 (9) | 0.0411 (7) | 0.1536 (5) | 0.040 (3) | |
H63 | 0.5041 | −0.0180 | 0.1354 | 0.048* | |
C64 | 0.4557 (9) | 0.0600 (8) | 0.1893 (5) | 0.041 (3) | |
H64 | 0.4005 | 0.0133 | 0.1967 | 0.050* | |
C65 | 0.4727 (8) | 0.1471 (7) | 0.2151 (4) | 0.032 (2) | |
H65 | 0.4277 | 0.1612 | 0.2387 | 0.038* | |
C66 | 0.5578 (8) | 0.2144 (7) | 0.2060 (4) | 0.026 (2) | |
H66 | 0.5712 | 0.2726 | 0.2250 | 0.031* | |
C67 | 0.6649 (7) | 0.3387 (6) | 0.0983 (3) | 0.0152 (18) | |
C68 | 0.5875 (7) | 0.2819 (6) | 0.0688 (3) | 0.022 (2) | |
H68 | 0.5627 | 0.2195 | 0.0781 | 0.027* | |
C69 | 0.5465 (8) | 0.3170 (7) | 0.0253 (3) | 0.027 (2) | |
H69 | 0.4932 | 0.2784 | 0.0060 | 0.033* | |
C70 | 0.5827 (7) | 0.4066 (7) | 0.0105 (3) | 0.025 (2) | |
H70 | 0.5532 | 0.4301 | −0.0183 | 0.030* | |
C71 | 0.6631 (8) | 0.4630 (7) | 0.0379 (3) | 0.023 (2) | |
H71 | 0.6898 | 0.5242 | 0.0271 | 0.027* | |
C72 | 0.7032 (7) | 0.4283 (6) | 0.0810 (3) | 0.0180 (19) | |
H72 | 0.7581 | 0.4664 | 0.0993 | 0.022* | |
C73 | 0.7233 (7) | 0.5150 (7) | 0.4236 (3) | 0.022 (2) | |
C74 | 0.6567 (7) | 0.4320 (7) | 0.4127 (3) | 0.025 (2) | |
H74 | 0.6250 | 0.4206 | 0.3793 | 0.029* | |
C75 | 0.6345 (8) | 0.3639 (7) | 0.4502 (4) | 0.029 (2) | |
H75 | 0.5884 | 0.3073 | 0.4418 | 0.035* | |
C76 | 0.6800 (9) | 0.3793 (8) | 0.4997 (4) | 0.038 (3) | |
H76 | 0.6659 | 0.3334 | 0.5250 | 0.045* | |
C77 | 0.7461 (8) | 0.4625 (8) | 0.5112 (4) | 0.034 (3) | |
H77 | 0.7768 | 0.4743 | 0.5449 | 0.040* | |
C78 | 0.7684 (8) | 0.5297 (8) | 0.4738 (3) | 0.031 (2) | |
H78 | 0.8147 | 0.5862 | 0.4823 | 0.038* | |
C79 | 0.8685 (8) | 0.6668 (8) | 0.3966 (3) | 0.033 (3) | |
C80 | 0.9387 (8) | 0.6126 (9) | 0.4014 (4) | 0.036 (3) | |
H80 | 0.9228 | 0.5484 | 0.3906 | 0.043* | |
C81 | 1.0321 (9) | 0.6534 (11) | 0.4219 (4) | 0.050 (4) | |
H81 | 1.0791 | 0.6166 | 0.4256 | 0.061* | |
C82 | 1.0562 (10) | 0.7480 (13) | 0.4371 (4) | 0.061 (5) | |
H82 | 1.1193 | 0.7756 | 0.4512 | 0.074* | |
C83 | 0.9885 (11) | 0.8012 (11) | 0.4314 (5) | 0.058 (4) | |
H83 | 1.0055 | 0.8657 | 0.4415 | 0.070* | |
C84 | 0.8959 (9) | 0.7623 (9) | 0.4112 (4) | 0.044 (3) | |
H84 | 0.8504 | 0.8006 | 0.4072 | 0.052* | |
C85 | 0.6812 (8) | 0.6903 (7) | 0.4011 (3) | 0.026 (2) | |
C86 | 0.6401 (9) | 0.6847 (8) | 0.4491 (4) | 0.034 (3) | |
H86 | 0.6423 | 0.6330 | 0.4699 | 0.041* | |
C87 | 0.5952 (10) | 0.7546 (9) | 0.4673 (4) | 0.046 (3) | |
H87 | 0.5671 | 0.7499 | 0.5002 | 0.055* | |
C88 | 0.5918 (11) | 0.8302 (9) | 0.4376 (5) | 0.053 (4) | |
H88 | 0.5606 | 0.8771 | 0.4498 | 0.063* | |
C89 | 0.6340 (10) | 0.8379 (8) | 0.3897 (4) | 0.044 (3) | |
H89 | 0.6327 | 0.8905 | 0.3695 | 0.053* | |
C90 | 0.6781 (8) | 0.7684 (7) | 0.3716 (4) | 0.033 (2) | |
H90 | 0.7066 | 0.7737 | 0.3389 | 0.039* | |
C91 | 0.4889 (7) | 0.4915 (7) | 0.3238 (3) | 0.020 (2) | |
C92 | 0.4433 (8) | 0.3976 (6) | 0.3104 (4) | 0.024 (2) | |
H92 | 0.4459 | 0.3734 | 0.2760 | 0.029* | |
C93 | 0.3941 (9) | 0.3395 (8) | 0.3476 (4) | 0.038 (3) | |
H93 | 0.3653 | 0.2758 | 0.3388 | 0.046* | |
C94 | 0.3881 (9) | 0.3767 (9) | 0.3979 (4) | 0.039 (3) | |
H94 | 0.3537 | 0.3383 | 0.4230 | 0.047* | |
C95 | 0.4307 (8) | 0.4664 (9) | 0.4110 (4) | 0.037 (3) | |
H95 | 0.4268 | 0.4904 | 0.4452 | 0.045* | |
C96 | 0.4812 (7) | 0.5253 (7) | 0.3739 (3) | 0.022 (2) | |
H96 | 0.5102 | 0.5885 | 0.3836 | 0.027* | |
C97 | 0.5264 (7) | 0.6764 (6) | 0.2804 (3) | 0.020 (2) | |
C98 | 0.4472 (8) | 0.6919 (7) | 0.3081 (4) | 0.033 (2) | |
H98 | 0.4158 | 0.6458 | 0.3304 | 0.040* | |
C99 | 0.4152 (9) | 0.7731 (8) | 0.3032 (5) | 0.043 (3) | |
H99 | 0.3614 | 0.7819 | 0.3220 | 0.052* | |
C100 | 0.4604 (9) | 0.8429 (7) | 0.2712 (5) | 0.041 (3) | |
H100 | 0.4397 | 0.8999 | 0.2690 | 0.049* | |
C101 | 0.5346 (9) | 0.8272 (7) | 0.2434 (4) | 0.033 (3) | |
H101 | 0.5636 | 0.8726 | 0.2201 | 0.040* | |
C102 | 0.5694 (7) | 0.7469 (7) | 0.2480 (4) | 0.025 (2) | |
H102 | 0.6232 | 0.7394 | 0.2288 | 0.030* | |
C103 | 0.4918 (7) | 0.5158 (6) | 0.2156 (3) | 0.0183 (19) | |
C104 | 0.4128 (8) | 0.5498 (7) | 0.1987 (4) | 0.028 (2) | |
H104 | 0.3973 | 0.6016 | 0.2166 | 0.034* | |
C105 | 0.3555 (9) | 0.5074 (7) | 0.1548 (4) | 0.035 (3) | |
H105 | 0.3005 | 0.5300 | 0.1437 | 0.042* | |
C106 | 0.3785 (8) | 0.4339 (8) | 0.1280 (4) | 0.035 (3) | |
H106 | 0.3406 | 0.4068 | 0.0978 | 0.042* | |
C107 | 0.4557 (8) | 0.3994 (9) | 0.1445 (4) | 0.040 (3) | |
H107 | 0.4701 | 0.3473 | 0.1264 | 0.048* | |
C108 | 0.5138 (8) | 0.4400 (7) | 0.1878 (4) | 0.031 (2) | |
H108 | 0.5682 | 0.4163 | 0.1985 | 0.037* | |
O1 | 0.2577 (14) | 0.1076 (12) | 0.0451 (7) | 0.065 (5)* | 0.50 |
C109 | 0.247 (2) | 0.0571 (18) | −0.0036 (7) | 0.103 (13)* | 0.50 |
H10A | 0.2620 | 0.1006 | −0.0320 | 0.123* | 0.50 |
H10B | 0.1794 | 0.0207 | −0.0095 | 0.123* | 0.50 |
C110 | 0.315 (3) | −0.0060 (19) | −0.0017 (9) | 0.115 (15)* | 0.50 |
H11A | 0.3770 | 0.0234 | −0.0163 | 0.137* | 0.50 |
H11B | 0.2869 | −0.0656 | −0.0213 | 0.137* | 0.50 |
C111 | 0.327 (2) | −0.0211 (17) | 0.0546 (11) | 0.092 (11)* | 0.50 |
H11C | 0.2772 | −0.0745 | 0.0654 | 0.110* | 0.50 |
H11D | 0.3920 | −0.0328 | 0.0632 | 0.110* | 0.50 |
C112 | 0.3160 (19) | 0.0673 (17) | 0.0798 (7) | 0.099 (12)* | 0.50 |
H11E | 0.2844 | 0.0552 | 0.1132 | 0.119* | 0.50 |
H11F | 0.3801 | 0.1101 | 0.0868 | 0.119* | 0.50 |
O2 | 0.139 (2) | 0.2160 (17) | 0.4205 (12) | 0.056 (9)* | 0.25 |
C113 | 0.041 (2) | 0.170 (2) | 0.4264 (15) | 0.060 (15)* | 0.25 |
H11G | 0.0017 | 0.1734 | 0.3945 | 0.072* | 0.25 |
H11H | 0.0144 | 0.1992 | 0.4557 | 0.072* | 0.25 |
C114 | 0.041 (2) | 0.0714 (19) | 0.4367 (14) | 0.036 (10)* | 0.25 |
H11I | 0.0294 | 0.0322 | 0.4042 | 0.044* | 0.25 |
H11J | −0.0096 | 0.0460 | 0.4611 | 0.044* | 0.25 |
C115 | 0.139 (3) | 0.076 (2) | 0.4603 (15) | 0.054 (13)* | 0.25 |
H11K | 0.1411 | 0.0868 | 0.4984 | 0.065* | 0.25 |
H11L | 0.1608 | 0.0174 | 0.4524 | 0.065* | 0.25 |
C116 | 0.2005 (18) | 0.156 (2) | 0.4355 (17) | 0.073 (18)* | 0.25 |
H11M | 0.2530 | 0.1889 | 0.4602 | 0.087* | 0.25 |
H11N | 0.2301 | 0.1336 | 0.4048 | 0.087* | 0.25 |
O3 | 0.512 (3) | 0.140 (2) | 0.3667 (13) | 0.062 (10)* | 0.25 |
C117 | 0.550 (3) | 0.103 (3) | 0.4113 (17) | 0.12 (3)* | 0.25 |
H11O | 0.5780 | 0.1533 | 0.4372 | 0.144* | 0.25 |
H11P | 0.6005 | 0.0696 | 0.4016 | 0.144* | 0.25 |
C118 | 0.468 (4) | 0.037 (4) | 0.4330 (15) | 0.08 (2)* | 0.25 |
H11Q | 0.4377 | 0.0683 | 0.4602 | 0.101* | 0.25 |
H11R | 0.4893 | −0.0168 | 0.4479 | 0.101* | 0.25 |
C119 | 0.399 (3) | 0.006 (3) | 0.387 (2) | 0.12 (3)* | 0.25 |
H11S | 0.4138 | −0.0488 | 0.3687 | 0.142* | 0.25 |
H11T | 0.3315 | −0.0098 | 0.3980 | 0.142* | 0.25 |
C120 | 0.416 (3) | 0.088 (3) | 0.3546 (15) | 0.055 (13)* | 0.25 |
H12A | 0.4078 | 0.0680 | 0.3174 | 0.066* | 0.25 |
H12B | 0.3690 | 0.1273 | 0.3620 | 0.066* | 0.25 |
O4 | 0.425 (2) | 0.0651 (16) | 0.0081 (12) | 0.053* | 0.25 |
C121 | 0.336 (3) | 0.058 (2) | 0.0325 (15) | 0.09 (2)* | 0.25 |
H12C | 0.3048 | 0.1090 | 0.0214 | 0.106* | 0.25 |
H12D | 0.3472 | 0.0641 | 0.0707 | 0.106* | 0.25 |
C122 | 0.2741 (19) | −0.034 (2) | 0.0167 (17) | 0.054* | 0.25 |
H12E | 0.2319 | −0.0293 | −0.0142 | 0.065* | 0.25 |
H12F | 0.2332 | −0.0597 | 0.0452 | 0.065* | 0.25 |
C123 | 0.345 (2) | −0.0917 (15) | 0.0045 (13) | 0.031 (9)* | 0.25 |
H12G | 0.3640 | −0.1214 | 0.0359 | 0.037* | 0.25 |
H12H | 0.3173 | −0.1409 | −0.0225 | 0.037* | 0.25 |
C124 | 0.428 (2) | −0.024 (2) | −0.0145 (13) | 0.050* | 0.25 |
H12I | 0.4893 | −0.0413 | −0.0041 | 0.060* | 0.25 |
H12J | 0.4228 | −0.0229 | −0.0528 | 0.060* | 0.25 |
O5 | −0.091 (3) | −0.012 (2) | 0.4486 (13) | 0.036 (9)* | 0.20 |
O6 | 0.383 (4) | −0.014 (3) | −0.0224 (18) | 0.057 (12)* | 0.20 |
O7 | 0.031 (4) | 0.138 (4) | 0.404 (2) | 0.040 (13)* | 0.15 |
O8 | 0.213 (3) | 0.169 (3) | 0.4069 (16) | 0.048 (10)* | 0.20 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1 | 0.0192 (6) | 0.0297 (5) | 0.0213 (5) | 0.0066 (4) | 0.0018 (3) | 0.0007 (4) |
Ru2 | 0.0188 (6) | 0.0296 (5) | 0.0224 (5) | 0.0063 (4) | 0.0013 (3) | 0.0022 (4) |
Ru3 | 0.0199 (6) | 0.0312 (5) | 0.0213 (5) | 0.0063 (4) | 0.0024 (4) | 0.0008 (4) |
Cl1 | 0.0112 (12) | 0.0212 (10) | 0.0142 (9) | 0.0070 (8) | 0.0024 (7) | −0.0002 (7) |
Cl2 | 0.0134 (13) | 0.0261 (11) | 0.0184 (10) | 0.0024 (8) | 0.0019 (8) | 0.0017 (8) |
Cl3 | 0.0188 (14) | 0.0213 (11) | 0.0170 (10) | 0.0071 (8) | 0.0029 (8) | −0.0017 (8) |
Cl4 | 0.0116 (13) | 0.0235 (11) | 0.0134 (9) | 0.0038 (8) | 0.0016 (7) | 0.0011 (8) |
S1 | 0.0121 (13) | 0.0161 (10) | 0.0125 (10) | 0.0048 (8) | 0.0008 (7) | 0.0001 (7) |
P1 | 0.0096 (14) | 0.0199 (11) | 0.0147 (10) | 0.0040 (8) | −0.0002 (8) | 0.0006 (8) |
P2 | 0.0104 (14) | 0.0194 (11) | 0.0129 (10) | 0.0055 (8) | 0.0005 (8) | −0.0001 (8) |
P3 | 0.0123 (14) | 0.0226 (12) | 0.0144 (10) | 0.0049 (9) | 0.0008 (8) | 0.0033 (8) |
P4 | 0.0075 (13) | 0.0187 (11) | 0.0146 (10) | 0.0029 (8) | −0.0007 (8) | 0.0021 (8) |
P5 | 0.0120 (14) | 0.0321 (13) | 0.0105 (10) | 0.0055 (9) | 0.0011 (8) | 0.0006 (9) |
P6 | 0.0108 (14) | 0.0242 (12) | 0.0133 (10) | 0.0036 (9) | 0.0015 (8) | 0.0008 (8) |
C1 | 0.021 (6) | 0.026 (5) | 0.016 (4) | 0.010 (4) | −0.002 (3) | 0.001 (3) |
C2 | 0.029 (7) | 0.031 (5) | 0.029 (5) | 0.006 (4) | 0.000 (4) | −0.003 (4) |
C3 | 0.044 (9) | 0.048 (7) | 0.033 (6) | 0.010 (6) | 0.007 (5) | −0.007 (5) |
C4 | 0.050 (9) | 0.036 (6) | 0.046 (7) | 0.007 (5) | 0.003 (6) | −0.014 (5) |
C5 | 0.043 (9) | 0.025 (6) | 0.058 (7) | 0.000 (5) | 0.008 (6) | −0.005 (5) |
C6 | 0.023 (7) | 0.024 (5) | 0.037 (6) | 0.007 (4) | 0.001 (4) | −0.001 (4) |
C7 | 0.018 (6) | 0.018 (4) | 0.024 (5) | 0.006 (4) | 0.007 (4) | 0.002 (3) |
C8 | 0.014 (6) | 0.033 (5) | 0.029 (5) | 0.005 (4) | −0.002 (4) | 0.008 (4) |
C9 | 0.020 (7) | 0.041 (6) | 0.038 (6) | 0.008 (4) | 0.005 (4) | 0.011 (5) |
C10 | 0.036 (9) | 0.041 (6) | 0.044 (7) | 0.015 (5) | 0.025 (5) | 0.009 (5) |
C11 | 0.026 (7) | 0.041 (6) | 0.017 (5) | 0.010 (4) | 0.006 (4) | 0.002 (4) |
C12 | 0.021 (6) | 0.023 (5) | 0.026 (5) | 0.007 (4) | 0.002 (4) | 0.001 (4) |
C13 | 0.012 (6) | 0.023 (5) | 0.025 (5) | 0.001 (4) | 0.003 (4) | 0.008 (4) |
C14 | 0.012 (6) | 0.032 (5) | 0.020 (5) | 0.002 (4) | −0.001 (3) | 0.002 (4) |
C15 | 0.011 (6) | 0.045 (6) | 0.028 (5) | 0.005 (4) | 0.001 (4) | 0.016 (4) |
C16 | 0.014 (6) | 0.041 (5) | 0.038 (5) | 0.007 (4) | −0.001 (4) | 0.017 (4) |
C17 | 0.021 (7) | 0.025 (5) | 0.049 (6) | 0.009 (4) | 0.002 (4) | 0.009 (4) |
C18 | 0.012 (6) | 0.022 (5) | 0.031 (5) | 0.010 (4) | −0.004 (4) | 0.006 (4) |
C19 | 0.011 (5) | 0.020 (4) | 0.015 (4) | 0.008 (3) | 0.001 (3) | 0.002 (3) |
C20 | 0.013 (6) | 0.027 (5) | 0.015 (4) | 0.010 (4) | −0.007 (3) | 0.001 (3) |
C21 | 0.018 (6) | 0.035 (5) | 0.015 (4) | 0.007 (4) | 0.001 (3) | 0.003 (4) |
C22 | 0.014 (7) | 0.034 (6) | 0.044 (6) | 0.015 (4) | 0.006 (4) | 0.008 (4) |
C23 | 0.019 (7) | 0.026 (6) | 0.071 (8) | 0.009 (4) | 0.003 (5) | 0.009 (5) |
C24 | 0.013 (6) | 0.016 (5) | 0.052 (6) | 0.005 (4) | 0.007 (4) | 0.001 (4) |
C25 | 0.014 (5) | 0.020 (4) | 0.022 (4) | 0.008 (3) | 0.001 (3) | 0.004 (3) |
C26 | 0.028 (7) | 0.025 (5) | 0.024 (5) | 0.008 (4) | −0.005 (4) | 0.000 (4) |
C27 | 0.027 (7) | 0.018 (5) | 0.047 (6) | 0.010 (4) | −0.012 (5) | −0.007 (4) |
C28 | 0.023 (7) | 0.020 (5) | 0.061 (7) | 0.008 (4) | 0.003 (5) | 0.005 (5) |
C29 | 0.025 (7) | 0.023 (5) | 0.050 (6) | −0.001 (4) | 0.011 (5) | 0.006 (4) |
C30 | 0.008 (6) | 0.022 (5) | 0.040 (6) | 0.003 (4) | 0.004 (4) | 0.002 (4) |
C31 | 0.019 (6) | 0.019 (4) | 0.015 (4) | 0.003 (4) | 0.004 (3) | −0.001 (3) |
C32 | 0.008 (5) | 0.025 (5) | 0.016 (4) | 0.007 (3) | 0.000 (3) | 0.005 (3) |
C33 | 0.022 (6) | 0.028 (5) | 0.014 (4) | 0.007 (4) | −0.003 (3) | 0.005 (3) |
C34 | 0.017 (6) | 0.037 (5) | 0.013 (4) | −0.002 (4) | −0.004 (3) | −0.004 (4) |
C35 | 0.022 (6) | 0.024 (5) | 0.021 (5) | 0.010 (4) | 0.004 (4) | −0.001 (4) |
C36 | 0.008 (5) | 0.021 (4) | 0.016 (4) | 0.006 (3) | −0.002 (3) | 0.001 (3) |
C37 | 0.008 (5) | 0.020 (4) | 0.023 (4) | 0.003 (3) | 0.004 (3) | 0.001 (3) |
C38 | 0.024 (6) | 0.012 (4) | 0.024 (5) | 0.001 (4) | 0.003 (4) | 0.004 (3) |
C39 | 0.024 (7) | 0.033 (5) | 0.034 (5) | 0.011 (4) | 0.011 (4) | 0.004 (4) |
C40 | 0.015 (7) | 0.030 (5) | 0.049 (6) | 0.014 (4) | 0.009 (4) | 0.007 (4) |
C41 | 0.026 (7) | 0.035 (6) | 0.042 (6) | 0.016 (5) | −0.006 (5) | 0.006 (5) |
C42 | 0.027 (7) | 0.029 (5) | 0.023 (5) | 0.006 (4) | −0.004 (4) | 0.001 (4) |
C43 | 0.023 (6) | 0.022 (5) | 0.016 (4) | 0.003 (4) | −0.002 (3) | 0.004 (3) |
C44 | 0.021 (7) | 0.036 (6) | 0.032 (5) | 0.005 (4) | 0.000 (4) | 0.003 (4) |
C45 | 0.030 (8) | 0.033 (6) | 0.046 (6) | 0.007 (5) | −0.002 (5) | 0.006 (5) |
C46 | 0.039 (9) | 0.025 (6) | 0.059 (7) | 0.004 (5) | −0.010 (5) | 0.005 (5) |
C47 | 0.018 (6) | 0.034 (5) | 0.050 (6) | −0.007 (4) | −0.001 (4) | 0.006 (4) |
C48 | 0.017 (7) | 0.030 (5) | 0.032 (5) | 0.005 (4) | −0.006 (4) | 0.009 (4) |
C49 | 0.023 (7) | 0.033 (5) | 0.017 (4) | 0.008 (4) | −0.004 (4) | 0.004 (4) |
C50 | 0.019 (7) | 0.044 (6) | 0.021 (5) | 0.003 (4) | 0.002 (4) | 0.007 (4) |
C51 | 0.033 (8) | 0.058 (8) | 0.033 (6) | −0.003 (6) | −0.013 (5) | 0.004 (5) |
C52 | 0.052 (10) | 0.078 (9) | 0.014 (5) | 0.010 (7) | −0.006 (5) | 0.007 (5) |
C53 | 0.046 (9) | 0.079 (9) | 0.015 (5) | 0.015 (6) | 0.005 (5) | 0.006 (5) |
C54 | 0.026 (7) | 0.046 (6) | 0.025 (5) | 0.005 (5) | 0.006 (4) | 0.006 (4) |
C55 | 0.016 (6) | 0.023 (5) | 0.016 (4) | 0.007 (4) | −0.002 (3) | 0.002 (3) |
C56 | 0.009 (6) | 0.023 (5) | 0.022 (4) | 0.009 (3) | 0.002 (3) | 0.001 (3) |
C57 | 0.015 (6) | 0.034 (5) | 0.025 (5) | 0.005 (4) | 0.003 (4) | 0.008 (4) |
C58 | 0.023 (7) | 0.029 (5) | 0.026 (5) | 0.013 (4) | 0.007 (4) | −0.001 (4) |
C59 | 0.017 (6) | 0.026 (5) | 0.031 (5) | 0.013 (4) | −0.003 (4) | 0.006 (4) |
C60 | 0.019 (6) | 0.031 (5) | 0.016 (4) | 0.014 (4) | 0.000 (3) | 0.006 (4) |
C61 | 0.016 (6) | 0.023 (5) | 0.017 (4) | 0.002 (4) | 0.001 (3) | 0.005 (3) |
C62 | 0.021 (7) | 0.026 (5) | 0.042 (6) | 0.013 (4) | −0.001 (4) | −0.001 (4) |
C63 | 0.023 (8) | 0.022 (5) | 0.074 (8) | 0.002 (4) | 0.003 (5) | 0.002 (5) |
C64 | 0.026 (8) | 0.034 (6) | 0.062 (8) | −0.002 (5) | 0.014 (5) | 0.005 (5) |
C65 | 0.008 (6) | 0.044 (6) | 0.043 (6) | 0.004 (4) | 0.005 (4) | 0.002 (5) |
C66 | 0.016 (6) | 0.029 (5) | 0.033 (5) | 0.007 (4) | −0.002 (4) | −0.004 (4) |
C67 | 0.008 (5) | 0.019 (4) | 0.020 (4) | 0.007 (3) | 0.004 (3) | −0.002 (3) |
C68 | 0.015 (6) | 0.025 (5) | 0.027 (5) | 0.006 (4) | −0.004 (4) | −0.003 (4) |
C69 | 0.027 (7) | 0.032 (5) | 0.020 (5) | 0.001 (4) | −0.006 (4) | −0.003 (4) |
C70 | 0.018 (6) | 0.041 (6) | 0.018 (5) | 0.011 (4) | −0.003 (4) | −0.001 (4) |
C71 | 0.023 (6) | 0.034 (5) | 0.016 (4) | 0.016 (4) | 0.004 (4) | 0.001 (4) |
C72 | 0.020 (6) | 0.025 (5) | 0.009 (4) | 0.005 (4) | 0.000 (3) | −0.002 (3) |
C73 | 0.011 (6) | 0.039 (6) | 0.019 (5) | 0.010 (4) | 0.006 (3) | 0.005 (4) |
C74 | 0.018 (6) | 0.035 (5) | 0.020 (5) | 0.004 (4) | 0.004 (4) | 0.004 (4) |
C75 | 0.022 (7) | 0.038 (6) | 0.029 (5) | 0.008 (4) | 0.005 (4) | 0.009 (4) |
C76 | 0.031 (8) | 0.061 (7) | 0.027 (5) | 0.018 (5) | 0.007 (4) | 0.024 (5) |
C77 | 0.021 (7) | 0.063 (7) | 0.016 (5) | 0.006 (5) | −0.003 (4) | 0.009 (4) |
C78 | 0.024 (7) | 0.055 (7) | 0.016 (5) | 0.010 (5) | 0.001 (4) | 0.006 (4) |
C79 | 0.018 (7) | 0.064 (7) | 0.011 (4) | −0.001 (5) | 0.001 (4) | −0.003 (4) |
C80 | 0.011 (7) | 0.072 (8) | 0.023 (5) | 0.009 (5) | 0.001 (4) | 0.001 (5) |
C81 | 0.017 (8) | 0.118 (12) | 0.017 (5) | 0.017 (7) | 0.002 (4) | 0.006 (6) |
C82 | 0.019 (9) | 0.125 (14) | 0.026 (6) | −0.014 (8) | 0.002 (5) | 0.007 (7) |
C83 | 0.042 (11) | 0.065 (9) | 0.049 (8) | −0.024 (7) | −0.012 (6) | −0.005 (6) |
C84 | 0.029 (8) | 0.059 (8) | 0.033 (6) | −0.010 (5) | −0.004 (5) | 0.004 (5) |
C85 | 0.020 (6) | 0.037 (6) | 0.017 (5) | 0.003 (4) | 0.000 (4) | −0.008 (4) |
C86 | 0.034 (8) | 0.043 (6) | 0.022 (5) | 0.005 (5) | 0.000 (4) | −0.003 (4) |
C87 | 0.046 (9) | 0.068 (8) | 0.028 (6) | 0.019 (6) | 0.017 (5) | −0.006 (5) |
C88 | 0.068 (11) | 0.057 (8) | 0.040 (7) | 0.029 (7) | 0.011 (6) | −0.014 (6) |
C89 | 0.066 (10) | 0.033 (6) | 0.042 (7) | 0.029 (6) | 0.007 (6) | −0.001 (5) |
C90 | 0.031 (7) | 0.038 (6) | 0.029 (5) | 0.009 (5) | 0.002 (4) | −0.002 (4) |
C91 | 0.011 (6) | 0.039 (5) | 0.014 (4) | 0.012 (4) | 0.000 (3) | 0.008 (4) |
C92 | 0.026 (7) | 0.019 (5) | 0.028 (5) | 0.006 (4) | 0.008 (4) | 0.005 (4) |
C93 | 0.023 (8) | 0.038 (6) | 0.055 (7) | 0.006 (5) | 0.002 (5) | 0.017 (5) |
C94 | 0.022 (7) | 0.064 (8) | 0.034 (6) | 0.010 (5) | 0.002 (4) | 0.022 (5) |
C95 | 0.020 (7) | 0.079 (9) | 0.014 (5) | 0.011 (5) | 0.007 (4) | 0.003 (5) |
C96 | 0.007 (6) | 0.033 (5) | 0.024 (5) | −0.003 (4) | 0.000 (3) | 0.002 (4) |
C97 | 0.009 (6) | 0.024 (5) | 0.026 (5) | 0.001 (4) | −0.004 (3) | −0.003 (4) |
C98 | 0.016 (7) | 0.028 (5) | 0.059 (7) | 0.008 (4) | 0.011 (5) | 0.000 (5) |
C99 | 0.027 (8) | 0.033 (6) | 0.073 (8) | 0.013 (5) | 0.010 (6) | −0.005 (5) |
C100 | 0.041 (9) | 0.023 (5) | 0.059 (7) | 0.009 (5) | −0.002 (6) | −0.002 (5) |
C101 | 0.033 (8) | 0.031 (6) | 0.034 (6) | 0.006 (5) | −0.011 (5) | 0.001 (4) |
C102 | 0.011 (6) | 0.040 (6) | 0.027 (5) | 0.010 (4) | −0.003 (4) | 0.000 (4) |
C103 | 0.015 (6) | 0.027 (5) | 0.011 (4) | 0.000 (4) | 0.000 (3) | 0.002 (3) |
C104 | 0.018 (7) | 0.031 (5) | 0.039 (6) | 0.015 (4) | −0.006 (4) | 0.000 (4) |
C105 | 0.027 (8) | 0.036 (6) | 0.040 (6) | 0.004 (5) | −0.017 (5) | 0.001 (5) |
C106 | 0.022 (7) | 0.055 (7) | 0.023 (5) | 0.002 (5) | −0.006 (4) | −0.005 (5) |
C107 | 0.013 (7) | 0.062 (8) | 0.042 (6) | 0.008 (5) | −0.004 (4) | −0.025 (5) |
C108 | 0.020 (7) | 0.043 (6) | 0.030 (5) | 0.011 (4) | −0.004 (4) | −0.010 (4) |
Ru1—P2 | 2.290 (2) | C59—C60 | 1.385 (13) |
Ru1—P1 | 2.378 (3) | C59—H59 | 0.9500 |
Ru1—S1 | 2.389 (2) | C60—H60 | 0.9500 |
Ru1—Cl3 | 2.459 (2) | C61—C66 | 1.377 (14) |
Ru1—Cl1 | 2.464 (2) | C61—C62 | 1.402 (13) |
Ru1—Cl4 | 2.495 (2) | C62—C63 | 1.416 (15) |
Ru2—P4 | 2.319 (2) | C62—H62 | 0.9500 |
Ru2—P3 | 2.371 (2) | C63—C64 | 1.356 (17) |
Ru2—Cl2 | 2.394 (2) | C63—H63 | 0.9500 |
Ru2—S1 | 2.408 (2) | C64—C65 | 1.391 (15) |
Ru2—Cl1 | 2.479 (2) | C64—H64 | 0.9500 |
Ru2—Cl4 | 2.536 (2) | C65—C66 | 1.415 (14) |
Ru3—P6 | 2.294 (3) | C65—H65 | 0.9500 |
Ru3—P5 | 2.372 (2) | C66—H66 | 0.9500 |
Ru3—S1 | 2.392 (2) | C67—C68 | 1.402 (13) |
Ru3—Cl2 | 2.409 (2) | C67—C72 | 1.404 (12) |
Ru3—Cl3 | 2.498 (2) | C68—C69 | 1.408 (13) |
Ru3—Cl4 | 2.530 (2) | C68—H68 | 0.9500 |
P1—C7 | 1.851 (9) | C69—C70 | 1.376 (14) |
P1—C1 | 1.854 (9) | C69—H69 | 0.9500 |
P1—C13 | 1.859 (9) | C70—C71 | 1.401 (14) |
P2—C25 | 1.836 (9) | C70—H70 | 0.9500 |
P2—C19 | 1.844 (9) | C71—C72 | 1.393 (13) |
P2—C31 | 1.877 (8) | C71—H71 | 0.9500 |
P3—C37 | 1.839 (9) | C72—H72 | 0.9500 |
P3—C43 | 1.860 (9) | C73—C74 | 1.380 (14) |
P3—C49 | 1.862 (9) | C73—C78 | 1.409 (13) |
P4—C55 | 1.842 (9) | C74—C75 | 1.410 (13) |
P4—C61 | 1.855 (9) | C74—H74 | 0.9500 |
P4—C67 | 1.871 (9) | C75—C76 | 1.396 (15) |
P5—C79 | 1.838 (11) | C75—H75 | 0.9500 |
P5—C85 | 1.843 (10) | C76—C77 | 1.381 (16) |
P5—C73 | 1.846 (9) | C76—H76 | 0.9500 |
P6—C97 | 1.832 (9) | C77—C78 | 1.399 (14) |
P6—C91 | 1.855 (9) | C77—H77 | 0.9500 |
P6—C103 | 1.869 (8) | C78—H78 | 0.9500 |
C1—C6 | 1.396 (14) | C79—C84 | 1.406 (16) |
C1—C2 | 1.398 (14) | C79—C80 | 1.411 (17) |
C2—C3 | 1.420 (15) | C80—C81 | 1.402 (16) |
C2—H2 | 0.9500 | C80—H80 | 0.9500 |
C3—C4 | 1.363 (17) | C81—C82 | 1.39 (2) |
C3—H3 | 0.9500 | C81—H81 | 0.9500 |
C4—C5 | 1.372 (17) | C82—C83 | 1.37 (2) |
C4—H4 | 0.9500 | C82—H82 | 0.9500 |
C5—C6 | 1.401 (14) | C83—C84 | 1.384 (18) |
C5—H5 | 0.9500 | C83—H83 | 0.9500 |
C6—H6 | 0.9500 | C84—H84 | 0.9500 |
C7—C12 | 1.389 (13) | C85—C86 | 1.388 (14) |
C7—C8 | 1.398 (14) | C85—C90 | 1.407 (15) |
C8—C9 | 1.383 (15) | C86—C87 | 1.400 (17) |
C8—H8 | 0.9500 | C86—H86 | 0.9500 |
C9—C10 | 1.384 (16) | C87—C88 | 1.381 (18) |
C9—H9 | 0.9500 | C87—H87 | 0.9500 |
C10—C11 | 1.374 (17) | C88—C89 | 1.394 (17) |
C10—H10 | 0.9500 | C88—H88 | 0.9500 |
C11—C12 | 1.396 (14) | C89—C90 | 1.388 (15) |
C11—H11 | 0.9500 | C89—H89 | 0.9500 |
C12—H12 | 0.9500 | C90—H90 | 0.9500 |
C13—C14 | 1.400 (13) | C91—C96 | 1.388 (13) |
C13—C18 | 1.412 (13) | C91—C92 | 1.414 (13) |
C14—C15 | 1.386 (14) | C92—C93 | 1.410 (14) |
C14—H14 | 0.9500 | C92—H92 | 0.9500 |
C15—C16 | 1.376 (15) | C93—C94 | 1.405 (17) |
C15—H15 | 0.9500 | C93—H93 | 0.9500 |
C16—C17 | 1.388 (15) | C94—C95 | 1.349 (17) |
C16—H16 | 0.9500 | C94—H94 | 0.9500 |
C17—C18 | 1.374 (13) | C95—C96 | 1.419 (14) |
C17—H17 | 0.9500 | C95—H95 | 0.9500 |
C18—H18 | 0.9500 | C96—H96 | 0.9500 |
C19—C24 | 1.395 (12) | C97—C102 | 1.401 (13) |
C19—C20 | 1.412 (13) | C97—C98 | 1.412 (14) |
C20—C21 | 1.379 (14) | C98—C99 | 1.375 (16) |
C20—H20 | 0.9500 | C98—H98 | 0.9500 |
C21—C22 | 1.381 (14) | C99—C100 | 1.399 (17) |
C21—H21 | 0.9500 | C99—H99 | 0.9500 |
C22—C23 | 1.394 (16) | C100—C101 | 1.354 (17) |
C22—H22 | 0.9500 | C100—H100 | 0.9500 |
C23—C24 | 1.374 (16) | C101—C102 | 1.383 (15) |
C23—H23 | 0.9500 | C101—H101 | 0.9500 |
C24—H24 | 0.9500 | C102—H102 | 0.9500 |
C25—C26 | 1.399 (13) | C103—C104 | 1.385 (14) |
C25—C30 | 1.402 (13) | C103—C108 | 1.404 (14) |
C26—C27 | 1.401 (14) | C104—C105 | 1.409 (14) |
C26—H26 | 0.9500 | C104—H104 | 0.9500 |
C27—C28 | 1.394 (16) | C105—C106 | 1.371 (16) |
C27—H27 | 0.9500 | C105—H105 | 0.9500 |
C28—C29 | 1.395 (15) | C106—C107 | 1.364 (17) |
C28—H28 | 0.9500 | C106—H106 | 0.9500 |
C29—C30 | 1.395 (13) | C107—C108 | 1.394 (14) |
C29—H29 | 0.9500 | C107—H107 | 0.9500 |
C30—H30 | 0.9500 | C108—H108 | 0.9500 |
C31—C36 | 1.397 (12) | O1—C112 | 1.4233 |
C31—C32 | 1.403 (12) | O1—C109 | 1.4234 |
C32—C33 | 1.389 (12) | C109—C110 | 1.4766 |
C32—H32 | 0.9500 | C109—H10A | 0.9900 |
C33—C34 | 1.376 (14) | C109—H10B | 0.9900 |
C33—H33 | 0.9500 | C110—C111 | 1.4888 |
C34—C35 | 1.394 (13) | C110—H11A | 0.9900 |
C34—H34 | 0.9500 | C110—H11B | 0.9900 |
C35—C36 | 1.396 (12) | C111—C112 | 1.4766 |
C35—H35 | 0.9500 | C111—H11C | 0.9900 |
C36—H36 | 0.9500 | C111—H11D | 0.9900 |
C37—C38 | 1.376 (12) | C112—H11E | 0.9900 |
C37—C42 | 1.407 (13) | C112—H11F | 0.9900 |
C38—C39 | 1.408 (14) | O2—C116 | 1.4233 |
C38—H38 | 0.9500 | O2—C113 | 1.4234 |
C39—C40 | 1.383 (15) | C113—C114 | 1.4766 |
C39—H39 | 0.9500 | C113—H11G | 0.9900 |
C40—C41 | 1.372 (15) | C113—H11H | 0.9900 |
C40—H40 | 0.9500 | C114—C115 | 1.4889 |
C41—C42 | 1.387 (16) | C114—H11I | 0.9900 |
C41—H41 | 0.9500 | C114—H11J | 0.9900 |
C42—H42 | 0.9500 | C115—C116 | 1.4766 |
C43—C48 | 1.368 (14) | C115—H11K | 0.9900 |
C43—C44 | 1.404 (14) | C115—H11L | 0.9900 |
C44—C45 | 1.392 (15) | C116—H11M | 0.9900 |
C44—H44 | 0.9500 | C116—H11N | 0.9900 |
C45—C46 | 1.379 (17) | O3—C117 | 1.4233 |
C45—H45 | 0.9500 | O3—C120 | 1.4233 |
C46—C47 | 1.407 (17) | C117—C118 | 1.4766 |
C46—H46 | 0.9500 | C117—H11O | 0.9900 |
C47—C48 | 1.384 (14) | C117—H11P | 0.9900 |
C47—H47 | 0.9500 | C118—C119 | 1.4888 |
C48—H48 | 0.9500 | C118—H11Q | 0.9900 |
C49—C50 | 1.403 (14) | C118—H11R | 0.9900 |
C49—C54 | 1.404 (14) | C119—C120 | 1.4766 |
C50—C51 | 1.376 (14) | C119—H11S | 0.9900 |
C50—H50 | 0.9500 | C119—H11T | 0.9900 |
C51—C52 | 1.401 (17) | C120—H12A | 0.9900 |
C51—H51 | 0.9500 | C120—H12B | 0.9900 |
C52—C53 | 1.357 (18) | O4—C121 | 1.4233 |
C52—H52 | 0.9500 | O4—C124 | 1.4234 |
C53—C54 | 1.389 (15) | C121—C122 | 1.4766 |
C53—H53 | 0.9500 | C121—H12C | 0.9900 |
C54—H54 | 0.9500 | C121—H12D | 0.9900 |
C55—C60 | 1.392 (12) | C122—C123 | 1.4889 |
C55—C56 | 1.397 (12) | C122—H12E | 0.9900 |
C56—C57 | 1.393 (13) | C122—H12F | 0.9900 |
C56—H56 | 0.9500 | C123—C124 | 1.4767 |
C57—C58 | 1.393 (13) | C123—H12G | 0.9900 |
C57—H57 | 0.9500 | C123—H12H | 0.9900 |
C58—C59 | 1.388 (14) | C124—H12I | 0.9900 |
C58—H58 | 0.9500 | C124—H12J | 0.9900 |
P2—Ru1—P1 | 98.04 (8) | C55—C56—H56 | 120.0 |
P2—Ru1—S1 | 94.42 (8) | C58—C57—C56 | 121.2 (8) |
P1—Ru1—S1 | 166.94 (8) | C58—C57—H57 | 119.4 |
P2—Ru1—Cl3 | 91.14 (8) | C56—C57—H57 | 119.4 |
P1—Ru1—Cl3 | 103.22 (8) | C59—C58—C57 | 118.6 (9) |
S1—Ru1—Cl3 | 80.36 (8) | C59—C58—H58 | 120.7 |
P2—Ru1—Cl1 | 104.52 (8) | C57—C58—H58 | 120.7 |
P1—Ru1—Cl1 | 92.62 (8) | C60—C59—C58 | 120.5 (8) |
S1—Ru1—Cl1 | 80.41 (8) | C60—C59—H59 | 119.7 |
Cl3—Ru1—Cl1 | 156.01 (8) | C58—C59—H59 | 119.7 |
P2—Ru1—Cl4 | 169.92 (9) | C59—C60—C55 | 121.2 (8) |
P1—Ru1—Cl4 | 90.02 (8) | C59—C60—H60 | 119.4 |
S1—Ru1—Cl4 | 78.03 (7) | C55—C60—H60 | 119.4 |
Cl3—Ru1—Cl4 | 81.09 (8) | C66—C61—C62 | 117.7 (9) |
Cl1—Ru1—Cl4 | 81.01 (7) | C66—C61—P4 | 118.5 (7) |
P4—Ru2—P3 | 96.70 (9) | C62—C61—P4 | 123.6 (7) |
P4—Ru2—Cl2 | 103.64 (9) | C61—C62—C63 | 121.3 (10) |
P3—Ru2—Cl2 | 94.21 (8) | C61—C62—H62 | 119.4 |
P4—Ru2—S1 | 96.17 (8) | C63—C62—H62 | 119.4 |
P3—Ru2—S1 | 166.98 (8) | C64—C63—C62 | 119.7 (10) |
Cl2—Ru2—S1 | 80.82 (8) | C64—C63—H63 | 120.2 |
P4—Ru2—Cl1 | 95.14 (8) | C62—C63—H63 | 120.2 |
P3—Ru2—Cl1 | 101.06 (8) | C63—C64—C65 | 120.6 (10) |
Cl2—Ru2—Cl1 | 154.22 (8) | C63—C64—H64 | 119.7 |
S1—Ru2—Cl1 | 79.73 (8) | C65—C64—H64 | 119.7 |
P4—Ru2—Cl4 | 172.04 (8) | C64—C65—C66 | 119.3 (10) |
P3—Ru2—Cl4 | 90.39 (8) | C64—C65—H65 | 120.3 |
Cl2—Ru2—Cl4 | 79.33 (8) | C66—C65—H65 | 120.3 |
S1—Ru2—Cl4 | 76.90 (8) | C61—C66—C65 | 121.4 (9) |
Cl1—Ru2—Cl4 | 79.90 (7) | C61—C66—H66 | 119.3 |
P6—Ru3—P5 | 96.56 (9) | C65—C66—H66 | 119.3 |
P6—Ru3—S1 | 93.96 (8) | C68—C67—C72 | 117.8 (8) |
P5—Ru3—S1 | 168.78 (9) | C68—C67—P4 | 121.7 (7) |
P6—Ru3—Cl2 | 93.07 (9) | C72—C67—P4 | 120.2 (7) |
P5—Ru3—Cl2 | 102.44 (8) | C67—C68—C69 | 120.2 (9) |
S1—Ru3—Cl2 | 80.84 (7) | C67—C68—H68 | 119.9 |
P6—Ru3—Cl3 | 105.48 (8) | C69—C68—H68 | 119.9 |
P5—Ru3—Cl3 | 93.86 (8) | C70—C69—C68 | 120.8 (9) |
S1—Ru3—Cl3 | 79.52 (7) | C70—C69—H69 | 119.6 |
Cl2—Ru3—Cl3 | 153.75 (8) | C68—C69—H69 | 119.6 |
P6—Ru3—Cl4 | 169.07 (8) | C69—C70—C71 | 120.0 (9) |
P5—Ru3—Cl4 | 92.66 (8) | C69—C70—H70 | 120.0 |
S1—Ru3—Cl4 | 77.31 (7) | C71—C70—H70 | 120.0 |
Cl2—Ru3—Cl4 | 79.18 (8) | C72—C71—C70 | 119.1 (9) |
Cl3—Ru3—Cl4 | 79.65 (8) | C72—C71—H71 | 120.5 |
Ru1—Cl1—Ru2 | 84.55 (7) | C70—C71—H71 | 120.5 |
Ru2—Cl2—Ru3 | 87.07 (7) | C71—C72—C67 | 122.0 (9) |
Ru1—Cl3—Ru3 | 84.20 (7) | C71—C72—H72 | 119.0 |
Ru1—Cl4—Ru3 | 82.81 (7) | C67—C72—H72 | 119.0 |
Ru1—Cl4—Ru2 | 82.73 (7) | C74—C73—C78 | 117.7 (9) |
Ru3—Cl4—Ru2 | 81.55 (7) | C74—C73—P5 | 120.0 (7) |
Ru1—S1—Ru3 | 88.06 (7) | C78—C73—P5 | 122.2 (8) |
Ru1—S1—Ru2 | 87.74 (8) | C73—C74—C75 | 121.4 (9) |
Ru3—S1—Ru2 | 87.13 (7) | C73—C74—H74 | 119.3 |
C7—P1—C1 | 102.2 (4) | C75—C74—H74 | 119.3 |
C7—P1—C13 | 96.2 (4) | C76—C75—C74 | 120.2 (10) |
C1—P1—C13 | 100.5 (4) | C76—C75—H75 | 119.9 |
C7—P1—Ru1 | 120.1 (3) | C74—C75—H75 | 119.9 |
C1—P1—Ru1 | 120.2 (3) | C77—C76—C75 | 118.8 (9) |
C13—P1—Ru1 | 113.4 (3) | C77—C76—H76 | 120.6 |
C25—P2—C19 | 99.8 (4) | C75—C76—H76 | 120.6 |
C25—P2—C31 | 101.0 (4) | C76—C77—C78 | 120.8 (9) |
C19—P2—C31 | 96.6 (4) | C76—C77—H77 | 119.6 |
C25—P2—Ru1 | 116.4 (3) | C78—C77—H77 | 119.6 |
C19—P2—Ru1 | 115.3 (3) | C77—C78—C73 | 121.0 (10) |
C31—P2—Ru1 | 123.5 (3) | C77—C78—H78 | 119.5 |
C37—P3—C43 | 99.9 (4) | C73—C78—H78 | 119.5 |
C37—P3—C49 | 101.1 (4) | C84—C79—C80 | 118.3 (10) |
C43—P3—C49 | 98.6 (4) | C84—C79—P5 | 125.0 (9) |
C37—P3—Ru2 | 120.6 (3) | C80—C79—P5 | 116.7 (9) |
C43—P3—Ru2 | 121.1 (3) | C81—C80—C79 | 120.1 (12) |
C49—P3—Ru2 | 111.8 (3) | C81—C80—H80 | 119.9 |
C55—P4—C61 | 103.0 (4) | C79—C80—H80 | 119.9 |
C55—P4—C67 | 97.7 (4) | C82—C81—C80 | 120.0 (13) |
C61—P4—C67 | 98.0 (4) | C82—C81—H81 | 120.0 |
C55—P4—Ru2 | 113.9 (3) | C80—C81—H81 | 120.0 |
C61—P4—Ru2 | 121.5 (3) | C83—C82—C81 | 119.8 (12) |
C67—P4—Ru2 | 118.8 (3) | C83—C82—H82 | 120.1 |
C79—P5—C85 | 97.1 (5) | C81—C82—H82 | 120.1 |
C79—P5—C73 | 99.4 (5) | C82—C83—C84 | 121.1 (14) |
C85—P5—C73 | 100.9 (4) | C82—C83—H83 | 119.5 |
C79—P5—Ru3 | 115.6 (3) | C84—C83—H83 | 119.5 |
C85—P5—Ru3 | 119.1 (3) | C83—C84—C79 | 120.6 (14) |
C73—P5—Ru3 | 120.5 (3) | C83—C84—H84 | 119.7 |
C97—P6—C91 | 104.9 (4) | C79—C84—H84 | 119.7 |
C97—P6—C103 | 97.8 (4) | C86—C85—C90 | 118.5 (10) |
C91—P6—C103 | 98.9 (4) | C86—C85—P5 | 124.3 (8) |
C97—P6—Ru3 | 120.0 (3) | C90—C85—P5 | 117.2 (7) |
C91—P6—Ru3 | 112.9 (3) | C85—C86—C87 | 120.7 (10) |
C103—P6—Ru3 | 119.3 (3) | C85—C86—H86 | 119.7 |
C6—C1—C2 | 118.3 (9) | C87—C86—H86 | 119.7 |
C6—C1—P1 | 124.6 (7) | C88—C87—C86 | 120.1 (10) |
C2—C1—P1 | 117.0 (7) | C88—C87—H87 | 119.9 |
C1—C2—C3 | 119.8 (10) | C86—C87—H87 | 119.9 |
C1—C2—H2 | 120.1 | C87—C88—C89 | 120.1 (11) |
C3—C2—H2 | 120.1 | C87—C88—H88 | 120.0 |
C4—C3—C2 | 120.3 (11) | C89—C88—H88 | 120.0 |
C4—C3—H3 | 119.8 | C90—C89—C88 | 119.7 (11) |
C2—C3—H3 | 119.8 | C90—C89—H89 | 120.1 |
C3—C4—C5 | 120.6 (10) | C88—C89—H89 | 120.1 |
C3—C4—H4 | 119.7 | C89—C90—C85 | 120.9 (10) |
C5—C4—H4 | 119.7 | C89—C90—H90 | 119.6 |
C4—C5—C6 | 120.0 (11) | C85—C90—H90 | 119.6 |
C4—C5—H5 | 120.0 | C96—C91—C92 | 118.2 (8) |
C6—C5—H5 | 120.0 | C96—C91—P6 | 121.3 (7) |
C1—C6—C5 | 120.9 (10) | C92—C91—P6 | 120.4 (7) |
C1—C6—H6 | 119.5 | C93—C92—C91 | 120.5 (9) |
C5—C6—H6 | 119.5 | C93—C92—H92 | 119.7 |
C12—C7—C8 | 118.0 (8) | C91—C92—H92 | 119.7 |
C12—C7—P1 | 122.1 (8) | C94—C93—C92 | 119.3 (10) |
C8—C7—P1 | 119.9 (7) | C94—C93—H93 | 120.4 |
C9—C8—C7 | 121.2 (9) | C92—C93—H93 | 120.4 |
C9—C8—H8 | 119.4 | C95—C94—C93 | 120.6 (10) |
C7—C8—H8 | 119.4 | C95—C94—H94 | 119.7 |
C8—C9—C10 | 119.8 (11) | C93—C94—H94 | 119.7 |
C8—C9—H9 | 120.1 | C94—C95—C96 | 120.6 (9) |
C10—C9—H9 | 120.1 | C94—C95—H95 | 119.7 |
C11—C10—C9 | 120.3 (9) | C96—C95—H95 | 119.7 |
C11—C10—H10 | 119.9 | C91—C96—C95 | 120.8 (9) |
C9—C10—H10 | 119.9 | C91—C96—H96 | 119.6 |
C10—C11—C12 | 119.8 (9) | C95—C96—H96 | 119.6 |
C10—C11—H11 | 120.1 | C102—C97—C98 | 116.9 (9) |
C12—C11—H11 | 120.1 | C102—C97—P6 | 118.4 (7) |
C7—C12—C11 | 121.0 (10) | C98—C97—P6 | 123.9 (7) |
C7—C12—H12 | 119.5 | C99—C98—C97 | 120.6 (10) |
C11—C12—H12 | 119.5 | C99—C98—H98 | 119.7 |
C14—C13—C18 | 118.5 (9) | C97—C98—H98 | 119.7 |
C14—C13—P1 | 123.6 (7) | C98—C99—C100 | 121.2 (12) |
C18—C13—P1 | 117.8 (7) | C98—C99—H99 | 119.4 |
C15—C14—C13 | 120.3 (9) | C100—C99—H99 | 119.4 |
C15—C14—H14 | 119.8 | C101—C100—C99 | 118.2 (10) |
C13—C14—H14 | 119.8 | C101—C100—H100 | 120.9 |
C16—C15—C14 | 120.7 (9) | C99—C100—H100 | 120.9 |
C16—C15—H15 | 119.6 | C100—C101—C102 | 122.0 (10) |
C14—C15—H15 | 119.6 | C100—C101—H101 | 119.0 |
C15—C16—C17 | 119.4 (9) | C102—C101—H101 | 119.0 |
C15—C16—H16 | 120.3 | C101—C102—C97 | 120.9 (10) |
C17—C16—H16 | 120.3 | C101—C102—H102 | 119.5 |
C18—C17—C16 | 121.0 (10) | C97—C102—H102 | 119.5 |
C18—C17—H17 | 119.5 | C104—C103—C108 | 118.8 (8) |
C16—C17—H17 | 119.5 | C104—C103—P6 | 120.7 (7) |
C17—C18—C13 | 119.9 (9) | C108—C103—P6 | 120.4 (8) |
C17—C18—H18 | 120.0 | C103—C104—C105 | 119.9 (10) |
C13—C18—H18 | 120.0 | C103—C104—H104 | 120.1 |
C24—C19—C20 | 118.3 (9) | C105—C104—H104 | 120.1 |
C24—C19—P2 | 123.3 (7) | C106—C105—C104 | 120.5 (11) |
C20—C19—P2 | 118.2 (6) | C106—C105—H105 | 119.8 |
C21—C20—C19 | 119.9 (8) | C104—C105—H105 | 119.8 |
C21—C20—H20 | 120.0 | C107—C106—C105 | 120.0 (10) |
C19—C20—H20 | 120.0 | C107—C106—H106 | 120.0 |
C20—C21—C22 | 120.9 (9) | C105—C106—H106 | 120.0 |
C20—C21—H21 | 119.6 | C106—C107—C108 | 120.8 (11) |
C22—C21—H21 | 119.6 | C106—C107—H107 | 119.6 |
C21—C22—C23 | 119.6 (10) | C108—C107—H107 | 119.6 |
C21—C22—H22 | 120.2 | C107—C108—C103 | 120.0 (11) |
C23—C22—H22 | 120.2 | C107—C108—H108 | 120.0 |
C24—C23—C22 | 120.0 (10) | C103—C108—H108 | 120.0 |
C24—C23—H23 | 120.0 | C112—O1—C109 | 108.8 |
C22—C23—H23 | 120.0 | O1—C109—C110 | 107.1 |
C23—C24—C19 | 121.1 (9) | O1—C109—H10A | 110.3 |
C23—C24—H24 | 119.4 | C110—C109—H10A | 110.3 |
C19—C24—H24 | 119.4 | O1—C109—H10B | 110.3 |
C26—C25—C30 | 117.2 (8) | C110—C109—H10B | 110.3 |
C26—C25—P2 | 118.6 (7) | H10A—C109—H10B | 108.6 |
C30—C25—P2 | 124.2 (7) | C109—C110—C111 | 103.6 |
C25—C26—C27 | 122.6 (9) | C109—C110—H11A | 111.0 |
C25—C26—H26 | 118.7 | C111—C110—H11A | 111.0 |
C27—C26—H26 | 118.7 | C109—C110—H11B | 111.0 |
C28—C27—C26 | 118.7 (9) | C111—C110—H11B | 111.0 |
C28—C27—H27 | 120.6 | H11A—C110—H11B | 109.0 |
C26—C27—H27 | 120.6 | C112—C111—C110 | 103.6 |
C27—C28—C29 | 120.0 (9) | C112—C111—H11C | 111.0 |
C27—C28—H28 | 120.0 | C110—C111—H11C | 111.0 |
C29—C28—H28 | 120.0 | C112—C111—H11D | 111.0 |
C30—C29—C28 | 120.3 (10) | C110—C111—H11D | 111.0 |
C30—C29—H29 | 119.9 | H11C—C111—H11D | 109.0 |
C28—C29—H29 | 119.9 | O1—C112—C111 | 107.1 |
C29—C30—C25 | 121.2 (9) | O1—C112—H11E | 110.3 |
C29—C30—H30 | 119.4 | C111—C112—H11E | 110.3 |
C25—C30—H30 | 119.4 | O1—C112—H11F | 110.3 |
C36—C31—C32 | 118.6 (7) | C111—C112—H11F | 110.3 |
C36—C31—P2 | 122.1 (7) | H11E—C112—H11F | 108.5 |
C32—C31—P2 | 119.3 (7) | C116—O2—C113 | 108.8 |
C33—C32—C31 | 120.1 (8) | O2—C113—C114 | 107.1 |
C33—C32—H32 | 119.9 | O2—C113—H11G | 110.3 |
C31—C32—H32 | 119.9 | C114—C113—H11G | 110.3 |
C34—C33—C32 | 121.4 (8) | O2—C113—H11H | 110.3 |
C34—C33—H33 | 119.3 | C114—C113—H11H | 110.3 |
C32—C33—H33 | 119.3 | H11G—C113—H11H | 108.6 |
C33—C34—C35 | 118.9 (8) | C113—C114—C115 | 103.6 |
C33—C34—H34 | 120.5 | C113—C114—H11I | 111.0 |
C35—C34—H34 | 120.5 | C115—C114—H11I | 111.0 |
C34—C35—C36 | 120.6 (8) | C113—C114—H11J | 111.0 |
C34—C35—H35 | 119.7 | C115—C114—H11J | 111.0 |
C36—C35—H35 | 119.7 | H11I—C114—H11J | 109.0 |
C35—C36—C31 | 120.3 (8) | C116—C115—C114 | 103.6 |
C35—C36—H36 | 119.8 | C116—C115—H11K | 111.0 |
C31—C36—H36 | 119.8 | C114—C115—H11K | 111.0 |
C38—C37—C42 | 119.0 (9) | C116—C115—H11L | 111.0 |
C38—C37—P3 | 119.1 (7) | C114—C115—H11L | 111.0 |
C42—C37—P3 | 121.6 (7) | H11K—C115—H11L | 109.0 |
C37—C38—C39 | 119.7 (9) | O2—C116—C115 | 107.1 |
C37—C38—H38 | 120.1 | O2—C116—H11M | 110.3 |
C39—C38—H38 | 120.1 | C115—C116—H11M | 110.3 |
C40—C39—C38 | 120.8 (9) | O2—C116—H11N | 110.3 |
C40—C39—H39 | 119.6 | C115—C116—H11N | 110.3 |
C38—C39—H39 | 119.6 | H11M—C116—H11N | 108.6 |
C41—C40—C39 | 119.5 (10) | C117—O3—C120 | 108.8 |
C41—C40—H40 | 120.3 | O3—C117—C118 | 107.1 |
C39—C40—H40 | 120.3 | O3—C117—H11O | 110.3 |
C40—C41—C42 | 120.4 (9) | C118—C117—H11O | 110.3 |
C40—C41—H41 | 119.8 | O3—C117—H11P | 110.3 |
C42—C41—H41 | 119.8 | C118—C117—H11P | 110.3 |
C41—C42—C37 | 120.6 (9) | H11O—C117—H11P | 108.6 |
C41—C42—H42 | 119.7 | C117—C118—C119 | 103.6 |
C37—C42—H42 | 119.7 | C117—C118—H11Q | 111.0 |
C48—C43—C44 | 117.7 (9) | C119—C118—H11Q | 111.0 |
C48—C43—P3 | 119.3 (7) | C117—C118—H11R | 111.0 |
C44—C43—P3 | 123.0 (8) | C119—C118—H11R | 111.0 |
C45—C44—C43 | 122.2 (11) | H11Q—C118—H11R | 109.0 |
C45—C44—H44 | 118.9 | C120—C119—C118 | 103.6 |
C43—C44—H44 | 118.9 | C120—C119—H11S | 111.0 |
C46—C45—C44 | 119.3 (11) | C118—C119—H11S | 111.0 |
C46—C45—H45 | 120.4 | C120—C119—H11T | 111.0 |
C44—C45—H45 | 120.4 | C118—C119—H11T | 111.0 |
C45—C46—C47 | 118.9 (10) | H11S—C119—H11T | 109.0 |
C45—C46—H46 | 120.6 | O3—C120—C119 | 107.1 |
C47—C46—H46 | 120.6 | O3—C120—H12A | 110.3 |
C48—C47—C46 | 120.8 (11) | C119—C120—H12A | 110.3 |
C48—C47—H47 | 119.6 | O3—C120—H12B | 110.3 |
C46—C47—H47 | 119.6 | C119—C120—H12B | 110.3 |
C43—C48—C47 | 121.2 (10) | H12A—C120—H12B | 108.6 |
C43—C48—H48 | 119.4 | C121—O4—C124 | 108.8 |
C47—C48—H48 | 119.4 | O4—C121—C122 | 107.1 |
C50—C49—C54 | 117.2 (9) | O4—C121—H12C | 110.3 |
C50—C49—P3 | 120.2 (7) | C122—C121—H12C | 110.3 |
C54—C49—P3 | 122.6 (8) | O4—C121—H12D | 110.3 |
C51—C50—C49 | 121.2 (9) | C122—C121—H12D | 110.3 |
C51—C50—H50 | 119.4 | H12C—C121—H12D | 108.6 |
C49—C50—H50 | 119.4 | C121—C122—C123 | 103.6 |
C50—C51—C52 | 120.1 (11) | C121—C122—H12E | 111.0 |
C50—C51—H51 | 120.0 | C123—C122—H12E | 111.0 |
C52—C51—H51 | 120.0 | C121—C122—H12F | 111.0 |
C53—C52—C51 | 119.7 (10) | C123—C122—H12F | 111.0 |
C53—C52—H52 | 120.2 | H12E—C122—H12F | 109.0 |
C51—C52—H52 | 120.2 | C124—C123—C122 | 103.6 |
C52—C53—C54 | 120.6 (11) | C124—C123—H12G | 111.0 |
C52—C53—H53 | 119.7 | C122—C123—H12G | 111.0 |
C54—C53—H53 | 119.7 | C124—C123—H12H | 111.0 |
C53—C54—C49 | 121.1 (11) | C122—C123—H12H | 111.0 |
C53—C54—H54 | 119.5 | H12G—C123—H12H | 109.0 |
C49—C54—H54 | 119.5 | O4—C124—C123 | 107.1 |
C60—C55—C56 | 118.5 (9) | O4—C124—H12I | 110.3 |
C60—C55—P4 | 122.0 (7) | C123—C124—H12I | 110.3 |
C56—C55—P4 | 119.1 (7) | O4—C124—H12J | 110.3 |
C57—C56—C55 | 119.9 (8) | C123—C124—H12J | 110.3 |
C57—C56—H56 | 120.0 | H12I—C124—H12J | 108.6 |
P2—Ru1—Cl1—Ru2 | −129.90 (8) | C31—P2—C19—C20 | 61.6 (7) |
P1—Ru1—Cl1—Ru2 | 131.10 (7) | Ru1—P2—C19—C20 | −70.4 (7) |
S1—Ru1—Cl1—Ru2 | −37.78 (7) | C24—C19—C20—C21 | 2.1 (12) |
Cl3—Ru1—Cl1—Ru2 | −0.7 (2) | P2—C19—C20—C21 | −173.2 (6) |
Cl4—Ru1—Cl1—Ru2 | 41.49 (7) | C19—C20—C21—C22 | 0.8 (13) |
P4—Ru2—Cl1—Ru1 | 132.88 (8) | C20—C21—C22—C23 | −2.5 (14) |
P3—Ru2—Cl1—Ru1 | −129.25 (8) | C21—C22—C23—C24 | 1.2 (16) |
Cl2—Ru2—Cl1—Ru1 | −4.1 (2) | C22—C23—C24—C19 | 1.8 (17) |
S1—Ru2—Cl1—Ru1 | 37.53 (7) | C20—C19—C24—C23 | −3.4 (14) |
Cl4—Ru2—Cl1—Ru1 | −40.84 (7) | P2—C19—C24—C23 | 171.7 (8) |
P4—Ru2—Cl2—Ru3 | −129.97 (8) | C19—P2—C25—C26 | 74.3 (8) |
P3—Ru2—Cl2—Ru3 | 132.08 (8) | C31—P2—C25—C26 | 173.1 (8) |
S1—Ru2—Cl2—Ru3 | −35.80 (7) | Ru1—P2—C25—C26 | −50.5 (8) |
Cl1—Ru2—Cl2—Ru3 | 5.6 (2) | C19—P2—C25—C30 | −105.0 (9) |
Cl4—Ru2—Cl2—Ru3 | 42.48 (7) | C31—P2—C25—C30 | −6.2 (9) |
P6—Ru3—Cl2—Ru2 | 129.60 (8) | Ru1—P2—C25—C30 | 130.2 (8) |
P5—Ru3—Cl2—Ru2 | −132.99 (8) | C30—C25—C26—C27 | 2.0 (15) |
S1—Ru3—Cl2—Ru2 | 36.08 (7) | P2—C25—C26—C27 | −177.3 (8) |
Cl3—Ru3—Cl2—Ru2 | −5.9 (2) | C25—C26—C27—C28 | −3.0 (16) |
Cl4—Ru3—Cl2—Ru2 | −42.63 (7) | C26—C27—C28—C29 | 2.4 (16) |
P2—Ru1—Cl3—Ru3 | 131.97 (8) | C27—C28—C29—C30 | −0.9 (17) |
P1—Ru1—Cl3—Ru3 | −129.50 (7) | C28—C29—C30—C25 | −0.1 (16) |
S1—Ru1—Cl3—Ru3 | 37.68 (7) | C26—C25—C30—C29 | −0.5 (15) |
Cl1—Ru1—Cl3—Ru3 | 0.5 (2) | P2—C25—C30—C29 | 178.8 (8) |
Cl4—Ru1—Cl3—Ru3 | −41.59 (7) | C25—P2—C31—C36 | 114.5 (8) |
P6—Ru3—Cl3—Ru1 | −128.99 (8) | C19—P2—C31—C36 | −144.1 (8) |
P5—Ru3—Cl3—Ru1 | 133.11 (8) | Ru1—P2—C31—C36 | −17.8 (9) |
S1—Ru3—Cl3—Ru1 | −37.75 (7) | C25—P2—C31—C32 | −64.8 (8) |
Cl2—Ru3—Cl3—Ru1 | 4.4 (2) | C19—P2—C31—C32 | 36.7 (8) |
Cl4—Ru3—Cl3—Ru1 | 41.11 (7) | Ru1—P2—C31—C32 | 163.0 (6) |
P2—Ru1—Cl4—Ru3 | 1.2 (5) | C36—C31—C32—C33 | 0.5 (14) |
P1—Ru1—Cl4—Ru3 | 144.48 (7) | P2—C31—C32—C33 | 179.7 (7) |
S1—Ru1—Cl4—Ru3 | −40.86 (7) | C31—C32—C33—C34 | 0.7 (14) |
Cl3—Ru1—Cl4—Ru3 | 41.09 (7) | C32—C33—C34—C35 | −0.8 (15) |
Cl1—Ru1—Cl4—Ru3 | −122.88 (7) | C33—C34—C35—C36 | −0.3 (15) |
P2—Ru1—Cl4—Ru2 | 83.5 (5) | C34—C35—C36—C31 | 1.5 (14) |
P1—Ru1—Cl4—Ru2 | −133.18 (8) | C32—C31—C36—C35 | −1.6 (14) |
S1—Ru1—Cl4—Ru2 | 41.48 (7) | P2—C31—C36—C35 | 179.2 (7) |
Cl3—Ru1—Cl4—Ru2 | 123.43 (8) | C43—P3—C37—C38 | 103.3 (7) |
Cl1—Ru1—Cl4—Ru2 | −40.54 (7) | C49—P3—C37—C38 | −155.8 (7) |
P6—Ru3—Cl4—Ru1 | 78.5 (4) | Ru2—P3—C37—C38 | −32.0 (8) |
P5—Ru3—Cl4—Ru1 | −133.96 (8) | C43—P3—C37—C42 | −70.2 (8) |
S1—Ru3—Cl4—Ru1 | 40.95 (7) | C49—P3—C37—C42 | 30.7 (8) |
Cl2—Ru3—Cl4—Ru1 | 123.88 (7) | Ru2—P3—C37—C42 | 154.5 (6) |
Cl3—Ru3—Cl4—Ru1 | −40.52 (6) | C42—C37—C38—C39 | 0.1 (13) |
P6—Ru3—Cl4—Ru2 | −5.2 (4) | P3—C37—C38—C39 | −173.6 (7) |
P5—Ru3—Cl4—Ru2 | 142.37 (7) | C37—C38—C39—C40 | 0.1 (14) |
S1—Ru3—Cl4—Ru2 | −42.73 (6) | C38—C39—C40—C41 | 0.5 (15) |
Cl2—Ru3—Cl4—Ru2 | 40.20 (6) | C39—C40—C41—C42 | −1.2 (16) |
Cl3—Ru3—Cl4—Ru2 | −124.19 (7) | C40—C41—C42—C37 | 1.4 (15) |
P4—Ru2—Cl4—Ru1 | −11.5 (6) | C38—C37—C42—C41 | −0.8 (14) |
P3—Ru2—Cl4—Ru1 | 141.55 (8) | P3—C37—C42—C41 | 172.7 (7) |
Cl2—Ru2—Cl4—Ru1 | −124.25 (8) | C37—P3—C43—C48 | −171.5 (7) |
S1—Ru2—Cl4—Ru1 | −41.30 (7) | C49—P3—C43—C48 | 85.6 (8) |
Cl1—Ru2—Cl4—Ru1 | 40.39 (7) | Ru2—P3—C43—C48 | −36.4 (8) |
P4—Ru2—Cl4—Ru3 | 72.2 (6) | C37—P3—C43—C44 | 10.0 (8) |
P3—Ru2—Cl4—Ru3 | −134.69 (7) | C49—P3—C43—C44 | −93.0 (8) |
Cl2—Ru2—Cl4—Ru3 | −40.49 (7) | Ru2—P3—C43—C44 | 145.0 (7) |
S1—Ru2—Cl4—Ru3 | 42.46 (7) | C48—C43—C44—C45 | −0.3 (14) |
Cl1—Ru2—Cl4—Ru3 | 124.15 (7) | P3—C43—C44—C45 | 178.3 (8) |
P2—Ru1—S1—Ru3 | −129.87 (8) | C43—C44—C45—C46 | 0.0 (16) |
P1—Ru1—S1—Ru3 | 67.7 (4) | C44—C45—C46—C47 | 0.3 (17) |
Cl3—Ru1—S1—Ru3 | −39.46 (7) | C45—C46—C47—C48 | −0.3 (17) |
Cl1—Ru1—S1—Ru3 | 126.13 (7) | C44—C43—C48—C47 | 0.3 (14) |
Cl4—Ru1—S1—Ru3 | 43.38 (7) | P3—C43—C48—C47 | −178.4 (8) |
P2—Ru1—S1—Ru2 | 142.93 (7) | C46—C47—C48—C43 | 0.0 (16) |
P1—Ru1—S1—Ru2 | −19.5 (4) | C37—P3—C49—C50 | 42.4 (9) |
Cl3—Ru1—S1—Ru2 | −126.66 (8) | C43—P3—C49—C50 | 144.3 (9) |
Cl1—Ru1—S1—Ru2 | 38.93 (7) | Ru2—P3—C49—C50 | −87.2 (9) |
Cl4—Ru1—S1—Ru2 | −43.82 (7) | C37—P3—C49—C54 | −138.8 (9) |
P6—Ru3—S1—Ru1 | 143.86 (8) | C43—P3—C49—C54 | −36.9 (10) |
P5—Ru3—S1—Ru1 | −15.7 (5) | Ru2—P3—C49—C54 | 91.6 (9) |
Cl2—Ru3—S1—Ru1 | −123.66 (8) | C54—C49—C50—C51 | 4.6 (16) |
Cl3—Ru3—S1—Ru1 | 38.84 (7) | P3—C49—C50—C51 | −176.5 (9) |
Cl4—Ru3—S1—Ru1 | −42.79 (7) | C49—C50—C51—C52 | −4.6 (19) |
P6—Ru3—S1—Ru2 | −128.30 (8) | C50—C51—C52—C53 | 2 (2) |
P5—Ru3—S1—Ru2 | 72.2 (5) | C51—C52—C53—C54 | 1 (2) |
Cl2—Ru3—S1—Ru2 | −35.83 (8) | C52—C53—C54—C49 | −1.3 (19) |
Cl3—Ru3—S1—Ru2 | 126.67 (8) | C50—C49—C54—C53 | −1.7 (17) |
Cl4—Ru3—S1—Ru2 | 45.04 (7) | P3—C49—C54—C53 | 179.5 (9) |
P4—Ru2—S1—Ru1 | −132.86 (8) | C61—P4—C55—C60 | −43.0 (9) |
P3—Ru2—S1—Ru1 | 55.9 (4) | C67—P4—C55—C60 | −143.1 (8) |
Cl2—Ru2—S1—Ru1 | 124.26 (8) | Ru2—P4—C55—C60 | 90.6 (8) |
Cl1—Ru2—S1—Ru1 | −38.73 (7) | C61—P4—C55—C56 | 143.7 (7) |
Cl4—Ru2—S1—Ru1 | 43.18 (7) | C67—P4—C55—C56 | 43.6 (8) |
P4—Ru2—S1—Ru3 | 138.97 (8) | Ru2—P4—C55—C56 | −82.7 (7) |
P3—Ru2—S1—Ru3 | −32.2 (4) | C60—C55—C56—C57 | 1.5 (14) |
Cl2—Ru2—S1—Ru3 | 36.09 (7) | P4—C55—C56—C57 | 175.1 (7) |
Cl1—Ru2—S1—Ru3 | −126.90 (8) | C55—C56—C57—C58 | 0.7 (14) |
Cl4—Ru2—S1—Ru3 | −44.99 (7) | C56—C57—C58—C59 | −0.9 (15) |
P2—Ru1—P1—C7 | −51.4 (3) | C57—C58—C59—C60 | −1.2 (15) |
S1—Ru1—P1—C7 | 110.9 (5) | C58—C59—C60—C55 | 3.5 (15) |
Cl3—Ru1—P1—C7 | −144.5 (3) | C56—C55—C60—C59 | −3.6 (14) |
Cl1—Ru1—P1—C7 | 53.6 (3) | P4—C55—C60—C59 | −176.9 (7) |
Cl4—Ru1—P1—C7 | 134.6 (3) | C55—P4—C61—C66 | 167.2 (8) |
P2—Ru1—P1—C1 | 76.9 (3) | C67—P4—C61—C66 | −92.9 (8) |
S1—Ru1—P1—C1 | −120.7 (4) | Ru2—P4—C61—C66 | 38.2 (9) |
Cl3—Ru1—P1—C1 | −16.2 (3) | C55—P4—C61—C62 | −18.4 (9) |
Cl1—Ru1—P1—C1 | −178.0 (3) | C67—P4—C61—C62 | 81.5 (8) |
Cl4—Ru1—P1—C1 | −97.0 (3) | Ru2—P4—C61—C62 | −147.3 (7) |
P2—Ru1—P1—C13 | −164.2 (3) | C66—C61—C62—C63 | −0.1 (15) |
S1—Ru1—P1—C13 | −1.8 (5) | P4—C61—C62—C63 | −174.7 (8) |
Cl3—Ru1—P1—C13 | 102.7 (3) | C61—C62—C63—C64 | 0.1 (18) |
Cl1—Ru1—P1—C13 | −59.1 (3) | C62—C63—C64—C65 | 1.8 (19) |
Cl4—Ru1—P1—C13 | 21.9 (3) | C63—C64—C65—C66 | −3.4 (18) |
P1—Ru1—P2—C25 | −23.7 (3) | C62—C61—C66—C65 | −1.6 (14) |
S1—Ru1—P2—C25 | 160.3 (3) | P4—C61—C66—C65 | 173.2 (8) |
Cl3—Ru1—P2—C25 | 79.9 (3) | C64—C65—C66—C61 | 3.4 (16) |
Cl1—Ru1—P2—C25 | −118.5 (3) | C55—P4—C67—C68 | 81.0 (8) |
Cl4—Ru1—P2—C25 | 119.2 (5) | C61—P4—C67—C68 | −23.4 (8) |
P1—Ru1—P2—C19 | −140.1 (3) | Ru2—P4—C67—C68 | −156.4 (7) |
S1—Ru1—P2—C19 | 43.8 (3) | C55—P4—C67—C72 | −93.0 (7) |
Cl3—Ru1—P2—C19 | −36.6 (3) | C61—P4—C67—C72 | 162.6 (7) |
Cl1—Ru1—P2—C19 | 125.0 (3) | Ru2—P4—C67—C72 | 29.7 (8) |
Cl4—Ru1—P2—C19 | 2.7 (6) | C72—C67—C68—C69 | −4.1 (14) |
P1—Ru1—P2—C31 | 102.1 (4) | P4—C67—C68—C69 | −178.2 (7) |
S1—Ru1—P2—C31 | −74.0 (4) | C67—C68—C69—C70 | 1.3 (15) |
Cl3—Ru1—P2—C31 | −154.4 (4) | C68—C69—C70—C71 | 1.9 (15) |
Cl1—Ru1—P2—C31 | 7.3 (4) | C69—C70—C71—C72 | −2.2 (14) |
Cl4—Ru1—P2—C31 | −115.1 (6) | C70—C71—C72—C67 | −0.7 (14) |
P4—Ru2—P3—C37 | 89.5 (3) | C68—C67—C72—C71 | 3.8 (13) |
Cl2—Ru2—P3—C37 | −166.2 (3) | P4—C67—C72—C71 | 178.0 (7) |
S1—Ru2—P3—C37 | −99.3 (5) | C79—P5—C73—C74 | −156.0 (9) |
Cl1—Ru2—P3—C37 | −7.1 (3) | C85—P5—C73—C74 | 104.8 (9) |
Cl4—Ru2—P3—C37 | −86.9 (3) | Ru3—P5—C73—C74 | −28.8 (10) |
P4—Ru2—P3—C43 | −36.5 (3) | C79—P5—C73—C78 | 27.6 (10) |
Cl2—Ru2—P3—C43 | 67.8 (3) | C85—P5—C73—C78 | −71.6 (9) |
S1—Ru2—P3—C43 | 134.7 (5) | Ru3—P5—C73—C78 | 154.8 (7) |
Cl1—Ru2—P3—C43 | −133.1 (3) | C78—C73—C74—C75 | −0.3 (15) |
Cl4—Ru2—P3—C43 | 147.1 (3) | P5—C73—C74—C75 | −176.9 (8) |
P4—Ru2—P3—C49 | −151.9 (4) | C73—C74—C75—C76 | 0.1 (16) |
Cl2—Ru2—P3—C49 | −47.6 (4) | C74—C75—C76—C77 | 0.6 (17) |
S1—Ru2—P3—C49 | 19.3 (6) | C75—C76—C77—C78 | −1.0 (18) |
Cl1—Ru2—P3—C49 | 111.5 (4) | C76—C77—C78—C73 | 0.8 (17) |
Cl4—Ru2—P3—C49 | 31.7 (4) | C74—C73—C78—C77 | −0.1 (16) |
P3—Ru2—P4—C55 | −51.7 (3) | P5—C73—C78—C77 | 176.4 (8) |
Cl2—Ru2—P4—C55 | −147.7 (3) | C85—P5—C79—C84 | −19.3 (9) |
S1—Ru2—P4—C55 | 130.3 (3) | C73—P5—C79—C84 | −121.6 (9) |
Cl1—Ru2—P4—C55 | 50.1 (3) | Ru3—P5—C79—C84 | 107.9 (8) |
Cl4—Ru2—P4—C55 | 101.2 (7) | C85—P5—C79—C80 | 157.7 (7) |
P3—Ru2—P4—C61 | 72.4 (4) | C73—P5—C79—C80 | 55.4 (8) |
Cl2—Ru2—P4—C61 | −23.6 (4) | Ru3—P5—C79—C80 | −75.2 (8) |
S1—Ru2—P4—C61 | −105.6 (4) | C84—C79—C80—C81 | 2.3 (14) |
Cl1—Ru2—P4—C61 | 174.2 (4) | P5—C79—C80—C81 | −174.9 (7) |
Cl4—Ru2—P4—C61 | −134.7 (7) | C79—C80—C81—C82 | −1.0 (15) |
P3—Ru2—P4—C67 | −165.9 (3) | C80—C81—C82—C83 | −0.5 (17) |
Cl2—Ru2—P4—C67 | 98.1 (3) | C81—C82—C83—C84 | 0.5 (19) |
S1—Ru2—P4—C67 | 16.1 (3) | C82—C83—C84—C79 | 0.8 (18) |
Cl1—Ru2—P4—C67 | −64.1 (3) | C80—C79—C84—C83 | −2.2 (15) |
Cl4—Ru2—P4—C67 | −13.0 (8) | P5—C79—C84—C83 | 174.7 (9) |
P6—Ru3—P5—C79 | −151.8 (4) | C79—P5—C85—C86 | −94.5 (9) |
S1—Ru3—P5—C79 | 7.7 (7) | C73—P5—C85—C86 | 6.5 (10) |
Cl2—Ru3—P5—C79 | 113.6 (4) | Ru3—P5—C85—C86 | 140.9 (8) |
Cl3—Ru3—P5—C79 | −45.7 (4) | C79—P5—C85—C90 | 82.3 (8) |
Cl4—Ru3—P5—C79 | 34.1 (4) | C73—P5—C85—C90 | −176.7 (8) |
P6—Ru3—P5—C85 | −36.7 (4) | Ru3—P5—C85—C90 | −42.3 (9) |
S1—Ru3—P5—C85 | 122.8 (5) | C90—C85—C86—C87 | 1.0 (17) |
Cl2—Ru3—P5—C85 | −131.3 (4) | P5—C85—C86—C87 | 177.8 (9) |
Cl3—Ru3—P5—C85 | 69.4 (4) | C85—C86—C87—C88 | 0 (2) |
Cl4—Ru3—P5—C85 | 149.2 (4) | C86—C87—C88—C89 | −1 (2) |
P6—Ru3—P5—C73 | 88.8 (4) | C87—C88—C89—C90 | 1 (2) |
S1—Ru3—P5—C73 | −111.8 (6) | C88—C89—C90—C85 | 0 (2) |
Cl2—Ru3—P5—C73 | −5.8 (4) | C86—C85—C90—C89 | −0.7 (16) |
Cl3—Ru3—P5—C73 | −165.1 (4) | P5—C85—C90—C89 | −177.8 (10) |
Cl4—Ru3—P5—C73 | −85.3 (4) | C97—P6—C91—C96 | −48.6 (9) |
P5—Ru3—P6—C97 | 70.6 (3) | C103—P6—C91—C96 | −149.1 (8) |
S1—Ru3—P6—C97 | −105.5 (3) | Ru3—P6—C91—C96 | 83.8 (8) |
Cl2—Ru3—P6—C97 | 173.5 (3) | C97—P6—C91—C92 | 135.3 (8) |
Cl3—Ru3—P6—C97 | −25.3 (3) | C103—P6—C91—C92 | 34.8 (9) |
Cl4—Ru3—P6—C97 | −142.1 (5) | Ru3—P6—C91—C92 | −92.3 (8) |
P5—Ru3—P6—C91 | −53.9 (3) | C96—C91—C92—C93 | −1.9 (15) |
S1—Ru3—P6—C91 | 130.1 (3) | P6—C91—C92—C93 | 174.3 (8) |
Cl2—Ru3—P6—C91 | 49.1 (3) | C91—C92—C93—C94 | 2.0 (16) |
Cl3—Ru3—P6—C91 | −149.7 (3) | C92—C93—C94—C95 | −1.5 (17) |
Cl4—Ru3—P6—C91 | 93.5 (5) | C93—C94—C95—C96 | 0.9 (18) |
P5—Ru3—P6—C103 | −169.3 (3) | C92—C91—C96—C95 | 1.2 (15) |
S1—Ru3—P6—C103 | 14.6 (3) | P6—C91—C96—C95 | −174.9 (8) |
Cl2—Ru3—P6—C103 | −66.4 (3) | C94—C95—C96—C91 | −0.8 (17) |
Cl3—Ru3—P6—C103 | 94.9 (3) | C91—P6—C97—C102 | −178.9 (7) |
Cl4—Ru3—P6—C103 | −22.0 (6) | C103—P6—C97—C102 | −77.5 (8) |
C7—P1—C1—C6 | 1.5 (10) | Ru3—P6—C97—C102 | 52.9 (8) |
C13—P1—C1—C6 | 100.2 (9) | C91—P6—C97—C98 | −8.8 (9) |
Ru1—P1—C1—C6 | −134.6 (8) | C103—P6—C97—C98 | 92.6 (9) |
C7—P1—C1—C2 | 179.0 (8) | Ru3—P6—C97—C98 | −137.0 (8) |
C13—P1—C1—C2 | −82.3 (8) | C102—C97—C98—C99 | −0.3 (15) |
Ru1—P1—C1—C2 | 42.9 (9) | P6—C97—C98—C99 | −170.6 (9) |
C6—C1—C2—C3 | −0.5 (15) | C97—C98—C99—C100 | −0.7 (19) |
P1—C1—C2—C3 | −178.1 (8) | C98—C99—C100—C101 | 2.5 (19) |
C1—C2—C3—C4 | −2.0 (18) | C99—C100—C101—C102 | −3.4 (17) |
C2—C3—C4—C5 | 4 (2) | C100—C101—C102—C97 | 2.5 (16) |
C3—C4—C5—C6 | −3 (2) | C98—C97—C102—C101 | −0.6 (14) |
C2—C1—C6—C5 | 1.3 (16) | P6—C97—C102—C101 | 170.3 (8) |
P1—C1—C6—C5 | 178.8 (8) | C97—P6—C103—C104 | −20.8 (8) |
C4—C5—C6—C1 | 0.3 (18) | C91—P6—C103—C104 | 85.7 (8) |
C1—P1—C7—C12 | −124.4 (7) | Ru3—P6—C103—C104 | −151.6 (7) |
C13—P1—C7—C12 | 133.4 (8) | C97—P6—C103—C108 | 163.2 (8) |
Ru1—P1—C7—C12 | 11.7 (9) | C91—P6—C103—C108 | −90.3 (8) |
C1—P1—C7—C8 | 58.0 (8) | Ru3—P6—C103—C108 | 32.3 (9) |
C13—P1—C7—C8 | −44.2 (8) | C108—C103—C104—C105 | 0.9 (15) |
Ru1—P1—C7—C8 | −165.9 (6) | P6—C103—C104—C105 | −175.2 (8) |
C12—C7—C8—C9 | 2.6 (14) | C103—C104—C105—C106 | −1.4 (16) |
P1—C7—C8—C9 | −179.7 (8) | C104—C105—C106—C107 | 1.9 (17) |
C7—C8—C9—C10 | −2.4 (15) | C105—C106—C107—C108 | −1.9 (18) |
C8—C9—C10—C11 | 0.9 (16) | C106—C107—C108—C103 | 1.4 (17) |
C9—C10—C11—C12 | 0.2 (16) | C104—C103—C108—C107 | −0.9 (15) |
C8—C7—C12—C11 | −1.5 (13) | P6—C103—C108—C107 | 175.2 (8) |
P1—C7—C12—C11 | −179.1 (7) | C112—O1—C109—C110 | −10.1 |
C10—C11—C12—C7 | 0.1 (15) | O1—C109—C110—C111 | 25.8 |
C7—P1—C13—C14 | 124.1 (8) | C109—C110—C111—C112 | −31.1 |
C1—P1—C13—C14 | 20.4 (9) | C109—O1—C112—C111 | −10.1 |
Ru1—P1—C13—C14 | −109.2 (8) | C110—C111—C112—O1 | 25.8 |
C7—P1—C13—C18 | −51.2 (8) | C116—O2—C113—C114 | −10.1 |
C1—P1—C13—C18 | −154.9 (8) | O2—C113—C114—C115 | 25.8 |
Ru1—P1—C13—C18 | 75.5 (8) | C113—C114—C115—C116 | −31.1 |
C18—C13—C14—C15 | 0.9 (14) | C113—O2—C116—C115 | −10.1 |
P1—C13—C14—C15 | −174.4 (8) | C114—C115—C116—O2 | 25.8 |
C13—C14—C15—C16 | 1.0 (15) | C120—O3—C117—C118 | −10.1 |
C14—C15—C16—C17 | −2.6 (16) | O3—C117—C118—C119 | 25.8 |
C15—C16—C17—C18 | 2.2 (16) | C117—C118—C119—C120 | −31.1 |
C16—C17—C18—C13 | −0.3 (16) | C117—O3—C120—C119 | −10.1 |
C14—C13—C18—C17 | −1.2 (14) | C118—C119—C120—O3 | 25.8 |
P1—C13—C18—C17 | 174.3 (8) | C124—O4—C121—C122 | −10.1 |
C25—P2—C19—C24 | −11.0 (8) | O4—C121—C122—C123 | 25.8 |
C31—P2—C19—C24 | −113.5 (8) | C121—C122—C123—C124 | −31.1 |
Ru1—P2—C19—C24 | 114.5 (7) | C121—O4—C124—C123 | −10.1 |
C25—P2—C19—C20 | 164.1 (6) | C122—C123—C124—O4 | 25.8 |
Experimental details
Crystal data | |
Chemical formula | [Ru3Cl4S(C18H15P)6]·1.25C4H8O·0.75H2O |
Mr | 2152.82 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 123 |
a, b, c (Å) | 14.183 (4), 14.699 (5), 25.814 (9) |
α, β, γ (°) | 91.904 (11), 92.328 (11), 102.784 (11) |
V (Å3) | 5239 (3) |
Z | 2 |
Radiation type | Synchrotron, λ = 0.55940 Å |
µ (mm−1) | 0.37 |
Crystal size (mm) | 0.08 × 0.03 × 0.02 |
Data collection | |
Diffractometer | SMART 6000 detector mounted on a Bruker Kappa Platform diffractometer |
Absorption correction | Multi-scan (SADABS; Blessings, 1995; Sheldrick, 1996) |
Tmin, Tmax | 0.987, 0.995 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 109758, 15139, 12160 |
Rint | 0.049 |
(sin θ/λ)max (Å−1) | 0.582 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.089, 0.243, 1.42 |
No. of reflections | 15139 |
No. of parameters | 1156 |
No. of restraints | 30 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.38, −1.25 |
Computer programs: SMART–KAPPA (Bruker, 2001), SAINT (Bruker, 2001), SAINT and XPREP (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), TEXSAN for Windows (Molecular Structure Corporation, 1997), Xtal3.6 (Hall et al., 1999), ORTEPII (Johnson, 1976) and WinGX (Farrugia, 1999).
It is now well established that the reaction of metal halide complexes with S[Si(CH3)3]2 produces metal sulfide clusters of high nuclearity. The ionic organometallic ruthenium sufide cluster complexes [Ru3S2(p-cymene)3]2+ (p-cymene is 4-isopropyltoluene) (Lockemeyer, Rauchfuss & Rheingold, 1989) and [{RuCl(TMT)}3S]+ (TMT is tetramethylthiophene) (Lockemeyer, Rauchfuss, Rheingold & Wilson, 1989) have been prepared via this method from [RuCl2(p-cymene)]2 and [RuCl2(TMT)]2, respectively. The neutral ruthenium sulfide clusters [Ru4S6(PPh3)4], [Ru5S6(PPh3)5] and [Ru6S8(PPh3)6] have been prepared from the reaction of [RuCl2(PPh3)3] with NaSH or S[Si(CH3)3]2 under various conditions (Eckermann et al., 2002).
Small crystals of the title molecule, (I), were isolated from the reaction of [RuCl2(PPh3)3] with S[Si(CH3)3]2, and is thought to be in an intermediate in the formation of halide free cluster compounds. The poorly diffracting crystals did not yield sufficient data on a conventional laboratory diffractometer. A single-crystal structure of (I) (Fig. 1) was eventually obtained using synchrotron radiation at the ChemMatCARS facility of the Advanced Photon Source.
The core of the cluster consists of a flat six-membered ring of alternating Ru and bridging chloro ligands. Additional µ3-capping chloro and sulfido ligands, one on each side of the six-membered ring, completes the core. Each Ru centre is coordinated by two PPh3 ligands and has distorted octahedral geometry with the βridging chloride occupying axial positions. Overall, the molecule has non-crystallographic C3v symmetry. A similar core geometry has been observed in the cationic cluster [Ru3Cl5((S)-binap)3]+ [binap is 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl] (Mashima et al., 1991), which has two µ3-chlorides capping a six-membered Ru3Cl3 ring. The cation of the organometallic ruthenium–sulfide cluster [{(TMT)RuCl}3S]+ also consists of a six-membered Ru3Cl3 ring which is capped by a µ3-S atom (Lockemeyer, Rauchfuss, Rheingold & Wilson, 1989). The bond distances of (I) are in accord with equivalent bond distances in these related clusters.