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
Key indicators
- Single-crystal synchrotron study
- T = 123 K
- Mean (C-C) = 0.015 Å
- Disorder in solvent or counterion
- R factor = 0.089
- wR factor = 0.243
- Data-to-parameter ratio = 13.1
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level A:
DIFF_020 Alert A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards.
Alert Level B:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 19.00 From the CIF: _reflns_number_total 15139 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 17306 Completeness (_total/calc) 87.48% Alert B: < 90% complete (theta max?)
Alert Level C:
THETM_01 Alert C The value of sine(theta_max)/wavelength is less than 0.590 Calculated sin(theta_max)/wavelength = 0.5820 PLAT_302 Alert C Anion/Solvent Disorder ....................... 31.00 Perc. PLAT_601 Alert C Structure Contains Solvent Accessible VOIDS of 78.00 A 3 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 51 P4 -RU2 -CL4 -RU1 -11.50 0.60 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 56 P4 -RU2 -CL4 -RU3 72.20 0.60 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 140 CL4 -RU2 -P4 -C55 101.20 0.70 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 145 CL4 -RU2 -P4 -C61 -134.70 0.70 1.555 1.555 1.555 1.555 PLAT_710 Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle # 150 CL4 -RU2 -P4 -C67 -13.00 0.80 1.555 1.555 1.555 1.555 PLAT_721 Alert C Bond Calc 1.49922, Rep 1.48880, Dev. 0.01 Ang. C118 -C119 1.555 1.555 General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C113 H100 Cl4 O2 P6 Ru3 S1 Atom count from _chemical_formula_moiety:C113 H101.5 Cl4 O2 P6 Ru3 S1 ABSMU_01 Radiation type not identified. Calculation of _exptl_absorpt_correction_mu not performed. REFLT_03 From the CIF: _diffrn_reflns_theta_max 19.00 From the CIF: _reflns_number_total 15139 From the CIF: _diffrn_reflns_limit_ max hkl 14. 16. 29. From the CIF: _diffrn_reflns_limit_ min hkl -14. -16. -29. TEST1: Expected hkl limits for theta max Calculated maximum hkl 16. 17. 30. Calculated minimum hkl -16. -17. -30. ALERT: Expected hkl max differ from CIF values
1 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
9 Alert Level C = Please check
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).
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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.