Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803010833/cv6193sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803010833/cv6193Isup2.hkl |
CCDC reference: 217362
A solution of [H2Ru3(CO)6(PCy3)3] (Süss-Fink et al., 1998) (127 mg, 0.1 mmol) in degassed cyclohexane (40 ml) is placed in a stainless-steel autoclave. After purging with hydrogen, the autoclave is pressurized with hydrogen (30 bar) and heated to 373 K. After 18 h, the autoclave is placed in an ice-bath and the pressure released. The solution is evaporated to dryness and the brown residue dissolved in dichloromethane (3 ml), before being chromatographed on a silica gel (100 GF254, Merck) column, using a mixture of hexane–CH2Cl2 (4:1) as eluant. The major red fraction gives [H4Ru4(CO)10(PCy3)2] in 30% yield. 1H NMR (200 MHz, CDCl3): δ −19.6 (s, 1H), −18.0 (s, 1H), −17.1 (s, 1H), −15.7 (s, 1H), 1.25 − 2.10 (m, 66H); 31P NMR (200 MHz, CDCl3): δ 57.3 (s, 1P), 53.2 (s, 1P). IR (cyclohexane, cm−1, CO): 2069 (w), 2062 (sh), 2022 (versus), 2003 (w), 1993 (s), 1982 (m), 1971 (w), 1966 (w). MS (ESI, m/z): 1248.0 Analysis calculated for C46H70O10P2Ru4: C 44.23, H 5.65%; found: C 43.66, H 5.62%. Red crystals of compound (I) were obtained at room temperature by slow evaporation of a CH3OH–CH2Cl2 (3:7) solution.
A red crystal of compound (I) was mounted at 153 K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using Mo Kα graphite monochromated radiation. Image plate distance 90 mm, ϕ oscillation scans 0–180°, step Δϕ = 1.0°, 2θ range 2.03–25.91°, dmax–dmin = 16.00–0.93 Å. The hydride ions were located from difference Fourier maps and fixed in their positions while the remaining H atoms were included in calculated positions and treated as riding atoms. One cyclohexyl group has been treated as disordered (C34–C36), with partial occupancy factors of 50/50.
Data collection: EXPOSE in IPDS Software (Stoe & Cie, 2000); cell refinement: CELL in IPDS Software; data reduction: INTEGRATE in IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.
Fig. 1. The molecular structure of (I) with the 50% probability displacement ellipsoids. The cyclohexyl groups and H atoms have been omitted for clarity. |
[Ru4H4(C18H33P)2(CO)10] | F(000) = 2528 |
Mr = 1249.24 | Dx = 1.510 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 12.461 (5) Å | Cell parameters from 7997 reflections |
b = 23.934 (5) Å | θ = 2.0–25.9° |
c = 18.541 (5) Å | µ = 1.19 mm−1 |
β = 96.545 (5)° | T = 153 K |
V = 5494 (3) Å3 | Block, red |
Z = 4 | 0.30 × 0.30 × 0.12 mm |
Stoe & Cie IPDS diffractometer | 10053 independent reflections |
Radiation source: fine-focus sealed tube | 6046 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.057 |
Detector resolution: 0 pixels mm-1 | θmax = 25.9°, θmin = 2.0° |
ϕ oscillation scans | h = −14→15 |
Absorption correction: empirical (using intensity measurements) (Walker & Stuart, 1983) | k = −29→29 |
Tmin = 0.641, Tmax = 0.895 | l = −20→20 |
38794 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.045 | H-atom parameters constrained |
S = 0.75 | w = 1/[σ2(Fo2) + (0.0085P)2] where P = (Fo2 + 2Fc2)/3 |
10053 reflections | (Δ/σ)max = 0.002 |
586 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.49 e Å−3 |
[Ru4H4(C18H33P)2(CO)10] | V = 5494 (3) Å3 |
Mr = 1249.24 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 12.461 (5) Å | µ = 1.19 mm−1 |
b = 23.934 (5) Å | T = 153 K |
c = 18.541 (5) Å | 0.30 × 0.30 × 0.12 mm |
β = 96.545 (5)° |
Stoe & Cie IPDS diffractometer | 10053 independent reflections |
Absorption correction: empirical (using intensity measurements) (Walker & Stuart, 1983) | 6046 reflections with I > 2σ(I) |
Tmin = 0.641, Tmax = 0.895 | Rint = 0.057 |
38794 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 0 restraints |
wR(F2) = 0.045 | H-atom parameters constrained |
S = 0.75 | Δρmax = 0.48 e Å−3 |
10053 reflections | Δρmin = −0.49 e Å−3 |
586 parameters |
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) | |
C1 | 0.3539 (3) | −0.05251 (16) | 0.4053 (2) | 0.0275 (10) | |
H1A | 0.4320 | −0.0425 | 0.4158 | 0.033* | |
C2 | 0.3270 (3) | −0.09186 (18) | 0.4669 (3) | 0.0385 (12) | |
H2A | 0.2500 | −0.1029 | 0.4588 | 0.046* | |
H2B | 0.3714 | −0.1262 | 0.4669 | 0.046* | |
C3 | 0.3497 (4) | −0.0623 (2) | 0.5401 (3) | 0.0514 (14) | |
H3A | 0.3318 | −0.0876 | 0.5791 | 0.062* | |
H3B | 0.4277 | −0.0533 | 0.5492 | 0.062* | |
C4 | 0.2846 (4) | −0.0090 (2) | 0.5422 (3) | 0.0592 (17) | |
H4A | 0.3033 | 0.0098 | 0.5895 | 0.071* | |
H4B | 0.2067 | −0.0183 | 0.5375 | 0.071* | |
C5 | 0.3067 (3) | 0.0303 (2) | 0.4815 (3) | 0.0530 (15) | |
H5A | 0.3821 | 0.0438 | 0.4904 | 0.064* | |
H5B | 0.2583 | 0.0631 | 0.4816 | 0.064* | |
C6 | 0.2894 (3) | 0.00213 (18) | 0.4067 (3) | 0.0413 (13) | |
H6A | 0.3121 | 0.0280 | 0.3696 | 0.050* | |
H6B | 0.2116 | −0.0059 | 0.3941 | 0.050* | |
C7 | 0.4479 (3) | −0.13859 (15) | 0.3188 (2) | 0.0253 (10) | |
H7 | 0.4690 | −0.1404 | 0.2684 | 0.030* | |
C8 | 0.5515 (3) | −0.12331 (16) | 0.3679 (3) | 0.0314 (10) | |
H8A | 0.5735 | −0.0849 | 0.3565 | 0.038* | |
H8B | 0.5366 | −0.1240 | 0.4192 | 0.038* | |
C9 | 0.6441 (3) | −0.16358 (17) | 0.3582 (3) | 0.0414 (13) | |
H9A | 0.6643 | −0.1598 | 0.3083 | 0.050* | |
H9B | 0.7078 | −0.1534 | 0.3925 | 0.050* | |
C10 | 0.6139 (3) | −0.22383 (17) | 0.3711 (3) | 0.0420 (12) | |
H10A | 0.6059 | −0.2292 | 0.4232 | 0.050* | |
H10B | 0.6726 | −0.2487 | 0.3587 | 0.050* | |
C11 | 0.5081 (3) | −0.23995 (17) | 0.3253 (3) | 0.0416 (12) | |
H11A | 0.5190 | −0.2398 | 0.2733 | 0.050* | |
H11B | 0.4870 | −0.2782 | 0.3383 | 0.050* | |
C12 | 0.4178 (3) | −0.19897 (16) | 0.3382 (2) | 0.0327 (10) | |
H12A | 0.4044 | −0.2006 | 0.3897 | 0.039* | |
H12B | 0.3504 | −0.2100 | 0.3080 | 0.039* | |
C13 | 0.3763 (3) | −0.03047 (15) | 0.2528 (2) | 0.0255 (10) | |
H13 | 0.3166 | −0.0023 | 0.2493 | 0.031* | |
C14 | 0.4803 (3) | 0.00215 (17) | 0.2789 (3) | 0.0409 (12) | |
H14A | 0.4758 | 0.0168 | 0.3284 | 0.049* | |
H14B | 0.5433 | −0.0232 | 0.2808 | 0.049* | |
C15 | 0.4950 (4) | 0.05082 (19) | 0.2270 (3) | 0.0598 (17) | |
H15A | 0.4346 | 0.0775 | 0.2282 | 0.072* | |
H15B | 0.5630 | 0.0707 | 0.2435 | 0.072* | |
C16 | 0.4985 (4) | 0.0308 (2) | 0.1500 (3) | 0.0615 (16) | |
H16A | 0.5631 | 0.0070 | 0.1477 | 0.074* | |
H16B | 0.5043 | 0.0633 | 0.1177 | 0.074* | |
C17 | 0.3977 (4) | −0.00232 (19) | 0.1240 (3) | 0.0496 (13) | |
H17A | 0.4035 | −0.0170 | 0.0747 | 0.059* | |
H17B | 0.3339 | 0.0226 | 0.1213 | 0.059* | |
C18 | 0.3826 (3) | −0.05074 (17) | 0.1753 (3) | 0.0390 (11) | |
H18A | 0.4438 | −0.0771 | 0.1750 | 0.047* | |
H18B | 0.3155 | −0.0711 | 0.1579 | 0.047* | |
C19 | −0.0732 (3) | −0.20077 (15) | 0.0399 (2) | 0.0235 (9) | |
H19 | −0.0904 | −0.2351 | 0.0099 | 0.028* | |
C20 | −0.1569 (3) | −0.15594 (15) | 0.0126 (2) | 0.0318 (11) | |
H20A | −0.2300 | −0.1690 | 0.0206 | 0.038* | |
H20B | −0.1417 | −0.1212 | 0.0408 | 0.038* | |
C21 | −0.1541 (4) | −0.14372 (18) | −0.0676 (3) | 0.0424 (12) | |
H21A | −0.1762 | −0.1775 | −0.0963 | 0.051* | |
H21B | −0.2062 | −0.1136 | −0.0828 | 0.051* | |
C22 | −0.0425 (4) | −0.12622 (17) | −0.0829 (3) | 0.0424 (12) | |
H22A | −0.0251 | −0.0894 | −0.0602 | 0.051* | |
H22B | −0.0416 | −0.1222 | −0.1360 | 0.051* | |
C23 | 0.0426 (4) | −0.16811 (17) | −0.0541 (3) | 0.0401 (12) | |
H23A | 0.1147 | −0.1532 | −0.0610 | 0.048* | |
H23B | 0.0318 | −0.2031 | −0.0825 | 0.048* | |
C24 | 0.0398 (3) | −0.18142 (15) | 0.0256 (2) | 0.0303 (10) | |
H24A | 0.0602 | −0.1478 | 0.0551 | 0.036* | |
H24B | 0.0930 | −0.2112 | 0.0405 | 0.036* | |
C25 | 0.0337 (3) | −0.26976 (14) | 0.1555 (2) | 0.0218 (9) | |
H25 | 0.0999 | −0.2467 | 0.1523 | 0.026* | |
C26 | 0.0406 (3) | −0.31716 (14) | 0.1003 (2) | 0.0275 (10) | |
H26A | −0.0192 | −0.3439 | 0.1039 | 0.033* | |
H26B | 0.0325 | −0.3015 | 0.0505 | 0.033* | |
C27 | 0.1485 (3) | −0.34773 (17) | 0.1143 (3) | 0.0368 (11) | |
H27A | 0.2077 | −0.3217 | 0.1061 | 0.044* | |
H27B | 0.1497 | −0.3790 | 0.0794 | 0.044* | |
C28 | 0.1679 (3) | −0.37062 (16) | 0.1917 (3) | 0.0385 (12) | |
H28A | 0.1148 | −0.4005 | 0.1980 | 0.046* | |
H28B | 0.2411 | −0.3871 | 0.2001 | 0.046* | |
C29 | 0.1570 (3) | −0.32422 (16) | 0.2470 (3) | 0.0372 (12) | |
H29A | 0.2160 | −0.2968 | 0.2448 | 0.045* | |
H29B | 0.1643 | −0.3404 | 0.2964 | 0.045* | |
C30 | 0.0478 (3) | −0.29433 (16) | 0.2324 (2) | 0.0303 (10) | |
H30A | −0.0113 | −0.3211 | 0.2379 | 0.036* | |
H30B | 0.0438 | −0.2640 | 0.2684 | 0.036* | |
C31 | −0.2034 (3) | −0.26581 (17) | 0.1314 (3) | 0.0324 (11) | |
H31 | −0.2583 | −0.2355 | 0.1213 | 0.039* | |
C32 | −0.2355 (4) | −0.28320 (18) | 0.2041 (3) | 0.0472 (14) | |
H32A | −0.1732 | −0.3023 | 0.2314 | 0.057* | |
H32B | −0.2502 | −0.2490 | 0.2314 | 0.057* | |
C33 | −0.3312 (4) | −0.3206 (2) | 0.2023 (3) | 0.0674 (17) | |
H33A | −0.3136 | −0.3502 | 0.2390 | 0.081* | |
H33B | −0.3911 | −0.2984 | 0.2184 | 0.081* | |
C34A | −0.3719 (10) | −0.3478 (5) | 0.1343 (7) | 0.065 (4) | 0.50 |
H34A | −0.4510 | −0.3520 | 0.1336 | 0.078* | 0.50 |
H34B | −0.3408 | −0.3859 | 0.1350 | 0.078* | 0.50 |
C35A | −0.3507 (13) | −0.3205 (8) | 0.0644 (13) | 0.050 (5) | 0.50 |
H35A | −0.4018 | −0.2891 | 0.0539 | 0.060* | 0.50 |
H35B | −0.3641 | −0.3479 | 0.0244 | 0.060* | 0.50 |
C36A | −0.2339 (7) | −0.2982 (4) | 0.0666 (5) | 0.039 (2) | 0.50 |
H36A | −0.1836 | −0.3301 | 0.0650 | 0.047* | 0.50 |
H36B | −0.2280 | −0.2747 | 0.0234 | 0.047* | 0.50 |
C34B | −0.4192 (7) | −0.3131 (4) | 0.1472 (6) | 0.038 (3) | 0.50 |
H34C | −0.4626 | −0.2807 | 0.1600 | 0.046* | 0.50 |
H34D | −0.4661 | −0.3466 | 0.1457 | 0.046* | 0.50 |
C35B | −0.3852 (14) | −0.3040 (8) | 0.0746 (12) | 0.041 (4) | 0.50 |
H35C | −0.4488 | −0.2941 | 0.0400 | 0.049* | 0.50 |
H35D | −0.3538 | −0.3389 | 0.0574 | 0.049* | 0.50 |
C36B | −0.3002 (6) | −0.2564 (3) | 0.0768 (5) | 0.031 (2) | 0.50 |
H36C | −0.2757 | −0.2526 | 0.0281 | 0.037* | 0.50 |
H36D | −0.3350 | −0.2208 | 0.0883 | 0.037* | 0.50 |
C40 | 0.1695 (3) | −0.17735 (16) | 0.3496 (2) | 0.0249 (10) | |
C41 | 0.2344 (3) | −0.16567 (15) | 0.2079 (3) | 0.0272 (10) | |
C42 | −0.1007 (3) | −0.18782 (14) | 0.2999 (2) | 0.0212 (10) | |
C43 | −0.2172 (3) | −0.12699 (15) | 0.1911 (2) | 0.0263 (10) | |
C44 | −0.0992 (3) | −0.00139 (15) | 0.1524 (2) | 0.0267 (10) | |
C45 | 0.0923 (3) | 0.02532 (16) | 0.2302 (2) | 0.0271 (10) | |
C46 | 0.0872 (3) | −0.03179 (16) | 0.0907 (3) | 0.0293 (10) | |
C47 | −0.1643 (3) | −0.03734 (15) | 0.2930 (2) | 0.0236 (9) | |
C48 | 0.0140 (3) | 0.00681 (16) | 0.3762 (2) | 0.0269 (10) | |
C49 | −0.0560 (3) | −0.09850 (15) | 0.4045 (2) | 0.0250 (10) | |
O1 | 0.1662 (2) | −0.20829 (12) | 0.39683 (18) | 0.0405 (8) | |
O2 | 0.2791 (2) | −0.18935 (12) | 0.16547 (18) | 0.0415 (8) | |
O3 | −0.11331 (19) | −0.21484 (10) | 0.34985 (16) | 0.0290 (7) | |
O4 | −0.3081 (2) | −0.11754 (11) | 0.17100 (18) | 0.0395 (8) | |
O5 | −0.1780 (2) | 0.02217 (12) | 0.13156 (19) | 0.0489 (9) | |
O6 | 0.1299 (2) | 0.06531 (11) | 0.25645 (17) | 0.0418 (8) | |
O7 | 0.1238 (2) | −0.02429 (12) | 0.03795 (19) | 0.0444 (8) | |
O8 | −0.2517 (2) | −0.02185 (11) | 0.27832 (16) | 0.0359 (8) | |
O9 | 0.0279 (2) | 0.04545 (11) | 0.41251 (19) | 0.0467 (9) | |
O10 | −0.0807 (2) | −0.12001 (12) | 0.45612 (18) | 0.0424 (8) | |
P1 | 0.33681 (7) | −0.08586 (4) | 0.31556 (6) | 0.0216 (2) | |
P2 | −0.08097 (8) | −0.22030 (4) | 0.13623 (6) | 0.0209 (2) | |
Ru1 | 0.16393 (2) | −0.124402 (12) | 0.273894 (19) | 0.01823 (8) | |
Ru2 | −0.07325 (2) | −0.144501 (11) | 0.219955 (19) | 0.01766 (8) | |
Ru3 | 0.03107 (2) | −0.038972 (11) | 0.182365 (19) | 0.02026 (8) | |
Ru4 | −0.02180 (2) | −0.059575 (11) | 0.321727 (19) | 0.01791 (8) | |
H1 | 0.1196 | −0.0768 | 0.3379 | 0.050* | |
H2 | 0.1532 | −0.0700 | 0.2065 | 0.050* | |
H3 | −0.0315 | −0.1012 | 0.1480 | 0.050* | |
H4 | 0.0594 | −0.1663 | 0.2369 | 0.050* |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0134 (19) | 0.041 (2) | 0.028 (3) | −0.0036 (16) | −0.0002 (17) | −0.0109 (19) |
C2 | 0.026 (2) | 0.060 (3) | 0.031 (3) | −0.014 (2) | 0.012 (2) | −0.013 (2) |
C3 | 0.043 (3) | 0.091 (4) | 0.023 (3) | −0.030 (3) | 0.014 (2) | −0.017 (3) |
C4 | 0.042 (3) | 0.095 (4) | 0.046 (4) | −0.032 (3) | 0.027 (3) | −0.047 (3) |
C5 | 0.032 (3) | 0.068 (3) | 0.062 (4) | −0.011 (2) | 0.014 (2) | −0.042 (3) |
C6 | 0.026 (2) | 0.054 (3) | 0.045 (4) | 0.001 (2) | 0.005 (2) | −0.029 (2) |
C7 | 0.019 (2) | 0.033 (2) | 0.024 (3) | 0.0075 (16) | 0.0022 (17) | −0.0007 (19) |
C8 | 0.018 (2) | 0.041 (2) | 0.034 (3) | 0.0026 (18) | −0.0010 (18) | 0.004 (2) |
C9 | 0.019 (2) | 0.059 (3) | 0.046 (4) | 0.0065 (19) | 0.000 (2) | 0.006 (2) |
C10 | 0.035 (3) | 0.048 (3) | 0.042 (4) | 0.017 (2) | 0.000 (2) | 0.000 (2) |
C11 | 0.037 (3) | 0.038 (2) | 0.048 (4) | 0.0157 (19) | −0.002 (2) | −0.007 (2) |
C12 | 0.022 (2) | 0.035 (2) | 0.040 (3) | 0.0059 (18) | −0.0022 (18) | 0.003 (2) |
C13 | 0.016 (2) | 0.029 (2) | 0.033 (3) | −0.0012 (16) | 0.0050 (17) | 0.0008 (19) |
C14 | 0.030 (2) | 0.039 (3) | 0.053 (4) | −0.0142 (19) | −0.001 (2) | 0.011 (2) |
C15 | 0.047 (3) | 0.047 (3) | 0.083 (6) | −0.024 (2) | −0.006 (3) | 0.019 (3) |
C16 | 0.051 (3) | 0.064 (3) | 0.072 (5) | −0.009 (3) | 0.015 (3) | 0.030 (3) |
C17 | 0.053 (3) | 0.057 (3) | 0.042 (4) | −0.006 (2) | 0.018 (3) | 0.013 (3) |
C18 | 0.040 (3) | 0.044 (3) | 0.036 (4) | −0.004 (2) | 0.014 (2) | 0.003 (2) |
C19 | 0.028 (2) | 0.0198 (18) | 0.021 (3) | 0.0016 (17) | −0.0021 (17) | −0.0044 (18) |
C20 | 0.036 (2) | 0.028 (2) | 0.029 (3) | 0.0061 (18) | −0.006 (2) | −0.0006 (19) |
C21 | 0.063 (3) | 0.035 (2) | 0.026 (3) | 0.008 (2) | −0.010 (2) | 0.002 (2) |
C22 | 0.070 (3) | 0.033 (2) | 0.023 (3) | 0.000 (2) | 0.002 (2) | 0.004 (2) |
C23 | 0.052 (3) | 0.043 (3) | 0.027 (4) | −0.001 (2) | 0.012 (2) | 0.005 (2) |
C24 | 0.038 (2) | 0.029 (2) | 0.023 (3) | 0.0043 (17) | 0.0023 (19) | 0.0013 (18) |
C25 | 0.020 (2) | 0.0200 (19) | 0.026 (3) | 0.0029 (15) | 0.0021 (17) | −0.0020 (17) |
C26 | 0.034 (2) | 0.021 (2) | 0.026 (3) | 0.0030 (16) | −0.0016 (19) | −0.0075 (17) |
C27 | 0.037 (2) | 0.031 (2) | 0.042 (4) | 0.0079 (19) | 0.002 (2) | −0.007 (2) |
C28 | 0.035 (2) | 0.032 (2) | 0.047 (4) | 0.0144 (19) | −0.002 (2) | −0.004 (2) |
C29 | 0.044 (3) | 0.035 (2) | 0.031 (3) | 0.0124 (19) | −0.005 (2) | −0.001 (2) |
C30 | 0.041 (2) | 0.024 (2) | 0.026 (3) | 0.0057 (19) | 0.0024 (19) | −0.004 (2) |
C31 | 0.024 (2) | 0.044 (3) | 0.028 (3) | −0.0064 (18) | 0.0015 (19) | −0.008 (2) |
C32 | 0.055 (3) | 0.046 (3) | 0.039 (4) | −0.024 (2) | −0.001 (2) | 0.000 (2) |
C33 | 0.057 (4) | 0.086 (4) | 0.062 (5) | −0.036 (3) | 0.018 (3) | −0.021 (3) |
C34A | 0.083 (9) | 0.065 (8) | 0.049 (9) | −0.057 (7) | 0.020 (7) | −0.024 (7) |
C35A | 0.047 (11) | 0.064 (11) | 0.037 (11) | −0.028 (8) | −0.007 (9) | −0.008 (8) |
C36A | 0.054 (6) | 0.044 (5) | 0.020 (6) | −0.015 (5) | 0.011 (4) | −0.012 (5) |
C34B | 0.028 (5) | 0.041 (6) | 0.045 (8) | −0.003 (4) | 0.002 (5) | −0.015 (5) |
C35B | 0.024 (7) | 0.059 (10) | 0.038 (10) | −0.011 (6) | 0.001 (6) | −0.021 (7) |
C36B | 0.030 (5) | 0.049 (5) | 0.013 (6) | −0.012 (4) | −0.006 (4) | −0.009 (4) |
C40 | 0.020 (2) | 0.031 (2) | 0.023 (3) | −0.0005 (17) | −0.0019 (18) | −0.002 (2) |
C41 | 0.025 (2) | 0.026 (2) | 0.030 (3) | −0.0044 (17) | 0.001 (2) | −0.0078 (19) |
C42 | 0.015 (2) | 0.017 (2) | 0.031 (3) | 0.0017 (15) | 0.0017 (18) | −0.0046 (18) |
C43 | 0.029 (2) | 0.029 (2) | 0.021 (3) | 0.0004 (18) | −0.0002 (19) | −0.0065 (18) |
C44 | 0.033 (2) | 0.028 (2) | 0.019 (3) | −0.0028 (18) | 0.0041 (19) | 0.0060 (18) |
C45 | 0.034 (2) | 0.028 (2) | 0.019 (3) | 0.0051 (18) | −0.0006 (19) | 0.0078 (18) |
C46 | 0.033 (2) | 0.027 (2) | 0.028 (3) | −0.0020 (18) | 0.003 (2) | 0.001 (2) |
C47 | 0.025 (2) | 0.026 (2) | 0.021 (3) | 0.0013 (18) | 0.0108 (18) | −0.0055 (18) |
C48 | 0.022 (2) | 0.026 (2) | 0.032 (3) | 0.0034 (17) | −0.0017 (18) | 0.002 (2) |
C49 | 0.036 (2) | 0.023 (2) | 0.016 (3) | 0.0042 (17) | 0.0004 (19) | −0.0043 (18) |
O1 | 0.0414 (18) | 0.0408 (19) | 0.038 (2) | −0.0036 (14) | −0.0034 (15) | 0.0148 (16) |
O2 | 0.0332 (17) | 0.051 (2) | 0.042 (2) | −0.0029 (14) | 0.0123 (15) | −0.0221 (16) |
O3 | 0.0312 (16) | 0.0286 (16) | 0.028 (2) | 0.0010 (11) | 0.0059 (13) | 0.0054 (13) |
O4 | 0.0272 (17) | 0.0428 (18) | 0.046 (2) | 0.0054 (13) | −0.0073 (15) | −0.0031 (15) |
O5 | 0.0357 (18) | 0.057 (2) | 0.054 (3) | 0.0181 (15) | 0.0059 (16) | 0.0183 (17) |
O6 | 0.059 (2) | 0.0237 (16) | 0.039 (2) | −0.0117 (14) | −0.0120 (15) | −0.0042 (14) |
O7 | 0.053 (2) | 0.052 (2) | 0.031 (3) | −0.0084 (15) | 0.0138 (17) | −0.0005 (16) |
O8 | 0.0227 (15) | 0.0529 (19) | 0.032 (2) | 0.0098 (13) | 0.0019 (13) | −0.0054 (14) |
O9 | 0.0462 (18) | 0.0287 (17) | 0.061 (3) | 0.0046 (13) | −0.0118 (16) | −0.0281 (16) |
O10 | 0.063 (2) | 0.0420 (18) | 0.023 (2) | −0.0037 (15) | 0.0087 (16) | 0.0049 (15) |
P1 | 0.0174 (5) | 0.0262 (5) | 0.0212 (7) | −0.0002 (4) | 0.0025 (4) | −0.0035 (4) |
P2 | 0.0229 (5) | 0.0178 (5) | 0.0215 (7) | 0.0016 (4) | −0.0002 (4) | −0.0028 (4) |
Ru1 | 0.01571 (15) | 0.01998 (15) | 0.0189 (2) | 0.00108 (12) | 0.00152 (13) | −0.00231 (14) |
Ru2 | 0.01794 (16) | 0.01648 (15) | 0.0181 (2) | 0.00068 (12) | 0.00008 (13) | −0.00206 (13) |
Ru3 | 0.02359 (17) | 0.01853 (15) | 0.0184 (2) | −0.00035 (13) | 0.00140 (13) | 0.00086 (14) |
Ru4 | 0.01733 (16) | 0.01826 (15) | 0.0180 (2) | 0.00146 (13) | 0.00153 (13) | −0.00295 (14) |
C1—C6 | 1.536 (5) | C26—H26A | 0.9900 |
C1—C2 | 1.546 (6) | C26—H26B | 0.9900 |
C1—P1 | 1.836 (4) | C27—C28 | 1.528 (6) |
C1—H1A | 1.0000 | C27—H27A | 0.9900 |
C2—C3 | 1.528 (6) | C27—H27B | 0.9900 |
C2—H2A | 0.9900 | C28—C29 | 1.528 (6) |
C2—H2B | 0.9900 | C28—H28A | 0.9900 |
C3—C4 | 1.514 (7) | C28—H28B | 0.9900 |
C3—H3A | 0.9900 | C29—C30 | 1.534 (5) |
C3—H3B | 0.9900 | C29—H29A | 0.9900 |
C4—C5 | 1.516 (7) | C29—H29B | 0.9900 |
C4—H4A | 0.9900 | C30—H30A | 0.9900 |
C4—H4B | 0.9900 | C30—H30B | 0.9900 |
C5—C6 | 1.534 (6) | C31—C36A | 1.444 (9) |
C5—H5A | 0.9900 | C31—C36B | 1.500 (9) |
C5—H5B | 0.9900 | C31—C32 | 1.507 (6) |
C6—H6A | 0.9900 | C31—P2 | 1.868 (4) |
C6—H6B | 0.9900 | C31—H31 | 1.0000 |
C7—C8 | 1.535 (5) | C32—C33 | 1.488 (6) |
C7—C12 | 1.546 (5) | C32—H32A | 0.9900 |
C7—P1 | 1.869 (3) | C32—H32B | 0.9900 |
C7—H7 | 1.0000 | C33—C34B | 1.421 (11) |
C8—C9 | 1.530 (5) | C33—C34A | 1.457 (11) |
C8—H8A | 0.9900 | C33—H33A | 0.9900 |
C8—H8B | 0.9900 | C33—H33B | 0.9900 |
C9—C10 | 1.516 (6) | C34A—C35A | 1.50 (3) |
C9—H9A | 0.9900 | C34A—H34A | 0.9900 |
C9—H9B | 0.9900 | C34A—H34B | 0.9900 |
C10—C11 | 1.533 (6) | C35A—C36A | 1.55 (2) |
C10—H10A | 0.9900 | C35A—H35A | 0.9900 |
C10—H10B | 0.9900 | C35A—H35B | 0.9900 |
C11—C12 | 1.532 (5) | C36A—H36A | 0.9900 |
C11—H11A | 0.9900 | C36A—H36B | 0.9900 |
C11—H11B | 0.9900 | C34B—C35B | 1.47 (3) |
C12—H12A | 0.9900 | C34B—H34C | 0.9900 |
C12—H12B | 0.9900 | C34B—H34D | 0.9900 |
C13—C18 | 1.527 (6) | C35B—C36B | 1.55 (2) |
C13—C14 | 1.542 (5) | C35B—H35C | 0.9900 |
C13—P1 | 1.866 (4) | C35B—H35D | 0.9900 |
C13—H13 | 1.0000 | C36B—H36C | 0.9900 |
C14—C15 | 1.536 (6) | C36B—H36D | 0.9900 |
C14—H14A | 0.9900 | C40—O1 | 1.151 (5) |
C14—H14B | 0.9900 | C40—Ru1 | 1.887 (4) |
C15—C16 | 1.511 (7) | C41—O2 | 1.162 (5) |
C15—H15A | 0.9900 | C41—Ru1 | 1.867 (4) |
C15—H15B | 0.9900 | C42—O3 | 1.154 (4) |
C16—C17 | 1.516 (6) | C42—Ru2 | 1.873 (4) |
C16—H16A | 0.9900 | C43—O4 | 1.173 (4) |
C16—H16B | 0.9900 | C43—Ru2 | 1.861 (4) |
C17—C18 | 1.524 (6) | C44—O5 | 1.159 (4) |
C17—H17A | 0.9900 | C44—Ru3 | 1.884 (4) |
C17—H17B | 0.9900 | C45—O6 | 1.149 (4) |
C18—H18A | 0.9900 | C45—Ru3 | 1.892 (4) |
C18—H18B | 0.9900 | C46—O7 | 1.140 (5) |
C19—C24 | 1.534 (5) | C46—Ru3 | 1.918 (5) |
C19—C20 | 1.540 (5) | C47—O8 | 1.152 (4) |
C19—P2 | 1.860 (4) | C47—Ru4 | 1.873 (4) |
C19—H19 | 1.0000 | C48—O9 | 1.146 (4) |
C20—C21 | 1.520 (6) | C48—Ru4 | 1.908 (4) |
C20—H20A | 0.9900 | C49—O10 | 1.159 (5) |
C20—H20B | 0.9900 | C49—Ru4 | 1.885 (5) |
C21—C22 | 1.509 (6) | P1—Ru1 | 2.3894 (12) |
C21—H21A | 0.9900 | P2—Ru2 | 2.3824 (11) |
C21—H21B | 0.9900 | Ru1—Ru4 | 3.0031 (9) |
C22—C23 | 1.512 (6) | Ru1—Ru3 | 3.0267 (7) |
C22—H22A | 0.9900 | Ru1—Ru2 | 3.0484 (12) |
C22—H22B | 0.9900 | Ru1—H1 | 1.7783 |
C23—C24 | 1.516 (6) | Ru1—H2 | 1.7988 |
C23—H23A | 0.9900 | Ru1—H4 | 1.7228 |
C23—H23B | 0.9900 | Ru2—Ru4 | 2.7977 (6) |
C24—H24A | 0.9900 | Ru2—Ru3 | 2.9600 (7) |
C24—H24B | 0.9900 | Ru2—H3 | 1.8110 |
C25—C30 | 1.535 (6) | Ru2—H4 | 1.7271 |
C25—C26 | 1.536 (5) | Ru3—Ru4 | 2.7824 (8) |
C25—P2 | 1.859 (3) | Ru3—H2 | 1.7063 |
C25—H25 | 1.0000 | Ru3—H3 | 1.7670 |
C26—C27 | 1.527 (5) | Ru4—H1 | 1.8006 |
C6—C1—C2 | 110.4 (3) | P2—C31—H31 | 97.1 |
C6—C1—P1 | 112.2 (3) | C33—C32—C31 | 116.1 (4) |
C2—C1—P1 | 113.1 (3) | C33—C32—H32A | 108.3 |
C6—C1—H1A | 106.9 | C31—C32—H32A | 108.3 |
C2—C1—H1A | 106.9 | C33—C32—H32B | 108.3 |
P1—C1—H1A | 106.9 | C31—C32—H32B | 108.3 |
C3—C2—C1 | 109.9 (4) | H32A—C32—H32B | 107.4 |
C3—C2—H2A | 109.7 | C34B—C33—C34A | 43.3 (6) |
C1—C2—H2A | 109.7 | C34B—C33—C32 | 119.5 (6) |
C3—C2—H2B | 109.7 | C34A—C33—C32 | 119.2 (6) |
C1—C2—H2B | 109.7 | C34B—C33—H33A | 132.5 |
H2A—C2—H2B | 108.2 | C34A—C33—H33A | 107.5 |
C4—C3—C2 | 111.6 (4) | C32—C33—H33A | 107.5 |
C4—C3—H3A | 109.3 | C34B—C33—H33B | 66.6 |
C2—C3—H3A | 109.3 | C34A—C33—H33B | 107.5 |
C4—C3—H3B | 109.3 | C32—C33—H33B | 107.5 |
C2—C3—H3B | 109.3 | H33A—C33—H33B | 107.0 |
H3A—C3—H3B | 108.0 | C33—C34A—C35A | 118.2 (10) |
C3—C4—C5 | 111.1 (4) | C33—C34A—H34A | 107.7 |
C3—C4—H4A | 109.4 | C35A—C34A—H34A | 107.8 |
C5—C4—H4A | 109.4 | C33—C34A—H34B | 107.7 |
C3—C4—H4B | 109.4 | C35A—C34A—H34B | 107.7 |
C5—C4—H4B | 109.4 | H34A—C34A—H34B | 107.1 |
H4A—C4—H4B | 108.0 | C34A—C35A—C36A | 112.6 (14) |
C4—C5—C6 | 112.4 (4) | C34A—C35A—H35A | 109.1 |
C4—C5—H5A | 109.1 | C36A—C35A—H35A | 109.1 |
C6—C5—H5A | 109.1 | C34A—C35A—H35B | 109.1 |
C4—C5—H5B | 109.1 | C36A—C35A—H35B | 109.1 |
C6—C5—H5B | 109.1 | H35A—C35A—H35B | 107.8 |
H5A—C5—H5B | 107.9 | C31—C36A—C35A | 111.4 (9) |
C5—C6—C1 | 111.7 (4) | C31—C36A—H36A | 109.3 |
C5—C6—H6A | 109.3 | C35A—C36A—H36A | 109.3 |
C1—C6—H6A | 109.3 | C31—C36A—H36B | 109.3 |
C5—C6—H6B | 109.3 | C35A—C36A—H36B | 109.3 |
C1—C6—H6B | 109.3 | H36A—C36A—H36B | 108.0 |
H6A—C6—H6B | 107.9 | C33—C34B—C35B | 113.3 (9) |
C8—C7—C12 | 107.2 (3) | C33—C34B—H34C | 108.9 |
C8—C7—P1 | 115.3 (3) | C35B—C34B—H34C | 108.9 |
C12—C7—P1 | 116.1 (2) | C33—C34B—H34D | 108.9 |
C8—C7—H7 | 105.8 | C35B—C34B—H34D | 108.9 |
C12—C7—H7 | 105.8 | H34C—C34B—H34D | 107.7 |
P1—C7—H7 | 105.8 | C34B—C35B—C36B | 110.5 (13) |
C9—C8—C7 | 112.0 (3) | C34B—C35B—H35C | 109.6 |
C9—C8—H8A | 109.2 | C36B—C35B—H35C | 109.6 |
C7—C8—H8A | 109.2 | C34B—C35B—H35D | 109.6 |
C9—C8—H8B | 109.2 | C36B—C35B—H35D | 109.6 |
C7—C8—H8B | 109.2 | H35C—C35B—H35D | 108.1 |
H8A—C8—H8B | 107.9 | C31—C36B—C35B | 113.7 (10) |
C10—C9—C8 | 112.1 (3) | C31—C36B—H36C | 108.8 |
C10—C9—H9A | 109.2 | C35B—C36B—H36C | 108.8 |
C8—C9—H9A | 109.2 | C31—C36B—H36D | 108.8 |
C10—C9—H9B | 109.2 | C35B—C36B—H36D | 108.8 |
C8—C9—H9B | 109.2 | H36C—C36B—H36D | 107.7 |
H9A—C9—H9B | 107.9 | O1—C40—Ru1 | 175.3 (3) |
C9—C10—C11 | 111.4 (4) | O2—C41—Ru1 | 177.2 (4) |
C9—C10—H10A | 109.4 | O3—C42—Ru2 | 177.3 (3) |
C11—C10—H10A | 109.4 | O4—C43—Ru2 | 177.4 (4) |
C9—C10—H10B | 109.4 | O5—C44—Ru3 | 177.5 (4) |
C11—C10—H10B | 109.4 | O6—C45—Ru3 | 177.2 (4) |
H10A—C10—H10B | 108.0 | O7—C46—Ru3 | 175.4 (4) |
C12—C11—C10 | 110.7 (3) | O8—C47—Ru4 | 176.5 (3) |
C12—C11—H11A | 109.5 | O9—C48—Ru4 | 173.7 (4) |
C10—C11—H11A | 109.5 | O10—C49—Ru4 | 176.2 (4) |
C12—C11—H11B | 109.5 | C1—P1—C13 | 104.16 (18) |
C10—C11—H11B | 109.5 | C1—P1—C7 | 104.77 (18) |
H11A—C11—H11B | 108.1 | C13—P1—C7 | 104.65 (18) |
C11—C12—C7 | 111.1 (3) | C1—P1—Ru1 | 117.90 (12) |
C11—C12—H12A | 109.4 | C13—P1—Ru1 | 111.39 (12) |
C7—C12—H12A | 109.4 | C7—P1—Ru1 | 112.78 (12) |
C11—C12—H12B | 109.4 | C25—P2—C19 | 102.79 (17) |
C7—C12—H12B | 109.4 | C25—P2—C31 | 104.10 (18) |
H12A—C12—H12B | 108.0 | C19—P2—C31 | 103.43 (19) |
C18—C13—C14 | 108.9 (3) | C25—P2—Ru2 | 112.76 (12) |
C18—C13—P1 | 114.0 (3) | C19—P2—Ru2 | 115.59 (12) |
C14—C13—P1 | 115.8 (3) | C31—P2—Ru2 | 116.56 (14) |
C18—C13—H13 | 105.7 | C41—Ru1—C40 | 98.74 (18) |
C14—C13—H13 | 105.7 | C41—Ru1—P1 | 86.69 (12) |
P1—C13—H13 | 105.7 | C40—Ru1—P1 | 93.62 (11) |
C15—C14—C13 | 110.1 (4) | C41—Ru1—Ru4 | 154.46 (12) |
C15—C14—H14A | 109.6 | C40—Ru1—Ru4 | 95.26 (12) |
C13—C14—H14A | 109.6 | P1—Ru1—Ru4 | 113.69 (3) |
C15—C14—H14B | 109.6 | C41—Ru1—Ru3 | 104.94 (13) |
C13—C14—H14B | 109.6 | C40—Ru1—Ru3 | 147.40 (11) |
H14A—C14—H14B | 108.2 | P1—Ru1—Ru3 | 109.62 (3) |
C16—C15—C14 | 111.7 (4) | Ru4—Ru1—Ru3 | 54.960 (18) |
C16—C15—H15A | 109.3 | C41—Ru1—Ru2 | 102.24 (12) |
C14—C15—H15A | 109.3 | C40—Ru1—Ru2 | 95.19 (11) |
C16—C15—H15B | 109.3 | P1—Ru1—Ru2 | 166.33 (3) |
C14—C15—H15B | 109.3 | Ru4—Ru1—Ru2 | 55.07 (2) |
H15A—C15—H15B | 107.9 | Ru3—Ru1—Ru2 | 58.316 (16) |
C15—C16—C17 | 110.7 (4) | C41—Ru1—H1 | 168.9 |
C15—C16—H16A | 109.5 | C40—Ru1—H1 | 85.5 |
C17—C16—H16A | 109.5 | P1—Ru1—H1 | 82.8 |
C15—C16—H16B | 109.5 | Ru4—Ru1—H1 | 33.2 |
C17—C16—H16B | 109.5 | Ru3—Ru1—H1 | 75.5 |
H16A—C16—H16B | 108.1 | Ru2—Ru1—H1 | 87.5 |
C16—C17—C18 | 110.9 (4) | C41—Ru1—H2 | 86.1 |
C16—C17—H17A | 109.5 | C40—Ru1—H2 | 175.2 |
C18—C17—H17A | 109.5 | P1—Ru1—H2 | 86.5 |
C16—C17—H17B | 109.5 | Ru4—Ru1—H2 | 80.3 |
C18—C17—H17B | 109.5 | Ru3—Ru1—H2 | 29.4 |
H17A—C17—H17B | 108.1 | Ru2—Ru1—H2 | 83.9 |
C17—C18—C13 | 111.6 (4) | H1—Ru1—H2 | 89.7 |
C17—C18—H18A | 109.3 | C41—Ru1—H4 | 79.7 |
C13—C18—H18A | 109.3 | C40—Ru1—H4 | 82.4 |
C17—C18—H18B | 109.3 | P1—Ru1—H4 | 165.1 |
C13—C18—H18B | 109.3 | Ru4—Ru1—H4 | 81.1 |
H18A—C18—H18B | 108.0 | Ru3—Ru1—H4 | 80.2 |
C24—C19—C20 | 109.5 (3) | Ru2—Ru1—H4 | 28.0 |
C24—C19—P2 | 113.0 (3) | H1—Ru1—H4 | 111.1 |
C20—C19—P2 | 112.5 (3) | H2—Ru1—H4 | 98.7 |
C24—C19—H19 | 107.2 | C43—Ru2—C42 | 95.43 (17) |
C20—C19—H19 | 107.2 | C43—Ru2—P2 | 91.06 (12) |
P2—C19—H19 | 107.2 | C42—Ru2—P2 | 95.56 (11) |
C21—C20—C19 | 111.4 (3) | C43—Ru2—Ru4 | 99.75 (12) |
C21—C20—H20A | 109.3 | C42—Ru2—Ru4 | 85.22 (11) |
C19—C20—H20A | 109.3 | P2—Ru2—Ru4 | 169.05 (3) |
C21—C20—H20B | 109.3 | C43—Ru2—Ru3 | 100.09 (12) |
C19—C20—H20B | 109.3 | C42—Ru2—Ru3 | 141.60 (11) |
H20A—C20—H20B | 108.0 | P2—Ru2—Ru3 | 118.85 (3) |
C22—C21—C20 | 111.2 (4) | Ru4—Ru2—Ru3 | 57.714 (18) |
C22—C21—H21A | 109.4 | C43—Ru2—Ru1 | 157.79 (11) |
C20—C21—H21A | 109.4 | C42—Ru2—Ru1 | 94.91 (11) |
C22—C21—H21B | 109.4 | P2—Ru2—Ru1 | 107.43 (3) |
C20—C21—H21B | 109.4 | Ru4—Ru2—Ru1 | 61.642 (11) |
H21A—C21—H21B | 108.0 | Ru3—Ru2—Ru1 | 60.475 (14) |
C21—C22—C23 | 111.9 (4) | C43—Ru2—H3 | 90.5 |
C21—C22—H22A | 109.2 | C42—Ru2—H3 | 173.5 |
C23—C22—H22A | 109.2 | P2—Ru2—H3 | 87.1 |
C21—C22—H22B | 109.2 | Ru4—Ru2—H3 | 91.1 |
C23—C22—H22B | 109.2 | Ru3—Ru2—H3 | 33.7 |
H22A—C22—H22B | 107.9 | Ru1—Ru2—H3 | 78.6 |
C22—C23—C24 | 113.0 (4) | C43—Ru2—H4 | 172.6 |
C22—C23—H23A | 109.0 | C42—Ru2—H4 | 86.9 |
C24—C23—H23A | 109.0 | P2—Ru2—H4 | 81.7 |
C22—C23—H23B | 109.0 | Ru4—Ru2—H4 | 87.4 |
C24—C23—H23B | 109.0 | Ru3—Ru2—H4 | 82.1 |
H23A—C23—H23B | 107.8 | Ru1—Ru2—H4 | 27.9 |
C23—C24—C19 | 110.8 (3) | H3—Ru2—H4 | 87.6 |
C23—C24—H24A | 109.5 | C44—Ru3—C45 | 92.15 (16) |
C19—C24—H24A | 109.5 | C44—Ru3—C46 | 94.89 (17) |
C23—C24—H24B | 109.5 | C45—Ru3—C46 | 100.00 (17) |
C19—C24—H24B | 109.5 | C44—Ru3—Ru4 | 94.07 (13) |
H24A—C24—H24B | 108.1 | C45—Ru3—Ru4 | 80.49 (13) |
C30—C25—C26 | 109.1 (3) | C46—Ru3—Ru4 | 171.00 (12) |
C30—C25—P2 | 115.2 (3) | C44—Ru3—Ru2 | 95.16 (11) |
C26—C25—P2 | 116.3 (3) | C45—Ru3—Ru2 | 138.42 (13) |
C30—C25—H25 | 105.0 | C46—Ru3—Ru2 | 119.97 (11) |
C26—C25—H25 | 105.0 | Ru4—Ru3—Ru2 | 58.216 (12) |
P2—C25—H25 | 105.0 | C44—Ru3—Ru1 | 152.36 (12) |
C27—C26—C25 | 110.8 (3) | C45—Ru3—Ru1 | 96.96 (11) |
C27—C26—H26A | 109.5 | C46—Ru3—Ru1 | 109.02 (12) |
C25—C26—H26A | 109.5 | Ru4—Ru3—Ru1 | 62.088 (18) |
C27—C26—H26B | 109.5 | Ru2—Ru3—Ru1 | 61.21 (2) |
C25—C26—H26B | 109.5 | C44—Ru3—H2 | 176.4 |
H26A—C26—H26B | 108.1 | C45—Ru3—H2 | 86.0 |
C26—C27—C28 | 111.9 (4) | C46—Ru3—H2 | 82.4 |
C26—C27—H27A | 109.2 | Ru4—Ru3—H2 | 88.7 |
C28—C27—H27A | 109.2 | Ru2—Ru3—H2 | 88.2 |
C26—C27—H27B | 109.2 | Ru1—Ru3—H2 | 31.2 |
C28—C27—H27B | 109.2 | C44—Ru3—H3 | 88.1 |
H27A—C27—H27B | 107.9 | C45—Ru3—H3 | 173.0 |
C29—C28—C27 | 110.7 (3) | C46—Ru3—H3 | 87.0 |
C29—C28—H28A | 109.5 | Ru4—Ru3—H3 | 92.5 |
C27—C28—H28A | 109.5 | Ru2—Ru3—H3 | 34.7 |
C29—C28—H28B | 109.5 | Ru1—Ru3—H3 | 79.8 |
C27—C28—H28B | 109.5 | H2—Ru3—H3 | 94.1 |
H28A—C28—H28B | 108.1 | C47—Ru4—C49 | 94.43 (17) |
C28—C29—C30 | 111.4 (3) | C47—Ru4—C48 | 94.08 (16) |
C28—C29—H29A | 109.3 | C49—Ru4—C48 | 92.39 (17) |
C30—C29—H29A | 109.3 | C47—Ru4—Ru3 | 90.15 (12) |
C28—C29—H29B | 109.3 | C49—Ru4—Ru3 | 160.56 (12) |
C30—C29—H29B | 109.3 | C48—Ru4—Ru3 | 106.14 (13) |
H29A—C29—H29B | 108.0 | C47—Ru4—Ru2 | 82.96 (12) |
C25—C30—C29 | 110.3 (3) | C49—Ru4—Ru2 | 97.72 (12) |
C25—C30—H30A | 109.6 | C48—Ru4—Ru2 | 169.65 (13) |
C29—C30—H30A | 109.6 | Ru3—Ru4—Ru2 | 64.070 (18) |
C25—C30—H30B | 109.6 | C47—Ru4—Ru1 | 143.19 (12) |
C29—C30—H30B | 109.6 | C49—Ru4—Ru1 | 103.79 (11) |
H30A—C30—H30B | 108.1 | C48—Ru4—Ru1 | 116.41 (11) |
C36A—C31—C36B | 53.4 (5) | Ru3—Ru4—Ru1 | 62.952 (13) |
C36A—C31—C32 | 121.6 (5) | Ru2—Ru4—Ru1 | 63.29 (2) |
C36B—C31—C32 | 111.7 (5) | C47—Ru4—H1 | 172.1 |
C36A—C31—P2 | 119.3 (4) | C49—Ru4—H1 | 93.4 |
C36B—C31—P2 | 122.3 (4) | C48—Ru4—H1 | 86.4 |
C32—C31—P2 | 114.7 (3) | Ru3—Ru4—H1 | 82.2 |
C36A—C31—H31 | 97.1 | Ru2—Ru4—H1 | 95.2 |
C36B—C31—H31 | 44.3 | Ru1—Ru4—H1 | 32.7 |
C32—C31—H31 | 97.1 | ||
C6—C1—C2—C3 | −56.7 (4) | C41—Ru1—Ru2—P2 | 13.65 (13) |
P1—C1—C2—C3 | 176.6 (3) | C40—Ru1—Ru2—P2 | −86.48 (13) |
C1—C2—C3—C4 | 58.5 (4) | P1—Ru1—Ru2—P2 | 143.60 (13) |
C2—C3—C4—C5 | −57.0 (5) | Ru4—Ru1—Ru2—P2 | −179.28 (3) |
C3—C4—C5—C6 | 53.8 (5) | Ru3—Ru1—Ru2—P2 | 113.79 (4) |
C4—C5—C6—C1 | −53.1 (5) | C41—Ru1—Ru2—Ru4 | −167.07 (13) |
C2—C1—C6—C5 | 54.2 (4) | C40—Ru1—Ru2—Ru4 | 92.80 (13) |
P1—C1—C6—C5 | −178.6 (3) | P1—Ru1—Ru2—Ru4 | −37.12 (13) |
C12—C7—C8—C9 | 58.3 (5) | Ru3—Ru1—Ru2—Ru4 | −66.93 (2) |
P1—C7—C8—C9 | −170.7 (3) | C41—Ru1—Ru2—Ru3 | −100.15 (13) |
C7—C8—C9—C10 | −56.0 (5) | C40—Ru1—Ru2—Ru3 | 159.73 (12) |
C8—C9—C10—C11 | 52.5 (5) | P1—Ru1—Ru2—Ru3 | 29.81 (13) |
C9—C10—C11—C12 | −53.9 (5) | Ru4—Ru1—Ru2—Ru3 | 66.93 (2) |
C10—C11—C12—C7 | 58.9 (5) | O5—C44—Ru3—C45 | 95 (8) |
C8—C7—C12—C11 | −60.1 (5) | O5—C44—Ru3—C46 | −5 (8) |
P1—C7—C12—C11 | 169.4 (3) | O5—C44—Ru3—Ru4 | 176 (100) |
C18—C13—C14—C15 | 57.1 (5) | O5—C44—Ru3—Ru2 | −126 (8) |
P1—C13—C14—C15 | −172.9 (3) | O5—C44—Ru3—Ru1 | −155 (8) |
C13—C14—C15—C16 | −57.4 (5) | O6—C45—Ru3—C44 | −73 (7) |
C14—C15—C16—C17 | 56.3 (5) | O6—C45—Ru3—C46 | 22 (7) |
C15—C16—C17—C18 | −55.7 (5) | O6—C45—Ru3—Ru4 | −167 (7) |
C16—C17—C18—C13 | 57.6 (5) | O6—C45—Ru3—Ru2 | −173 (7) |
C14—C13—C18—C17 | −57.9 (4) | O6—C45—Ru3—Ru1 | 133 (7) |
P1—C13—C18—C17 | 171.1 (3) | O7—C46—Ru3—C44 | 92 (5) |
C24—C19—C20—C21 | 57.5 (4) | O7—C46—Ru3—C45 | −1 (5) |
P2—C19—C20—C21 | −176.0 (3) | O7—C46—Ru3—Ru4 | −94 (5) |
C19—C20—C21—C22 | −56.4 (4) | O7—C46—Ru3—Ru2 | −169 (5) |
C20—C21—C22—C23 | 53.4 (5) | O7—C46—Ru3—Ru1 | −102 (5) |
C21—C22—C23—C24 | −53.2 (5) | C43—Ru2—Ru3—C44 | 3.63 (19) |
C22—C23—C24—C19 | 54.6 (5) | C42—Ru2—Ru3—C44 | −108.7 (2) |
C20—C19—C24—C23 | −55.9 (4) | P2—Ru2—Ru3—C44 | 100.49 (14) |
P2—C19—C24—C23 | 177.9 (3) | Ru4—Ru2—Ru3—C44 | −91.59 (13) |
C30—C25—C26—C27 | −58.4 (4) | Ru1—Ru2—Ru3—C44 | −164.86 (13) |
P2—C25—C26—C27 | 169.3 (3) | C43—Ru2—Ru3—C45 | 102.8 (2) |
C25—C26—C27—C28 | 56.6 (5) | C42—Ru2—Ru3—C45 | −9.5 (2) |
C26—C27—C28—C29 | −54.1 (5) | P2—Ru2—Ru3—C45 | −160.38 (17) |
C27—C28—C29—C30 | 54.7 (5) | Ru4—Ru2—Ru3—C45 | 7.54 (16) |
C26—C25—C30—C29 | 59.0 (4) | Ru1—Ru2—Ru3—C45 | −65.73 (16) |
P2—C25—C30—C29 | −168.1 (3) | C43—Ru2—Ru3—C46 | −95.05 (18) |
C28—C29—C30—C25 | −58.0 (5) | C42—Ru2—Ru3—C46 | 152.7 (2) |
C36A—C31—C32—C33 | −22.6 (8) | P2—Ru2—Ru3—C46 | 1.80 (14) |
C36B—C31—C32—C33 | 36.8 (6) | Ru4—Ru2—Ru3—C46 | 169.73 (13) |
P2—C31—C32—C33 | −178.6 (4) | Ru1—Ru2—Ru3—C46 | 96.45 (13) |
C31—C32—C33—C34B | −36.2 (8) | C43—Ru2—Ru3—Ru4 | 95.22 (13) |
C31—C32—C33—C34A | 13.8 (10) | C42—Ru2—Ru3—Ru4 | −17.07 (16) |
C34B—C33—C34A—C35A | 77.3 (14) | P2—Ru2—Ru3—Ru4 | −167.92 (3) |
C32—C33—C34A—C35A | −25.9 (16) | Ru1—Ru2—Ru3—Ru4 | −73.271 (17) |
C33—C34A—C35A—C36A | 43.2 (18) | C43—Ru2—Ru3—Ru1 | 168.49 (13) |
C36B—C31—C36A—C35A | −54.8 (11) | C42—Ru2—Ru3—Ru1 | 56.20 (16) |
C32—C31—C36A—C35A | 40.0 (12) | P2—Ru2—Ru3—Ru1 | −94.65 (3) |
P2—C31—C36A—C35A | −165.1 (10) | Ru4—Ru2—Ru3—Ru1 | 73.271 (17) |
C34A—C35A—C36A—C31 | −48.6 (15) | C41—Ru1—Ru3—C44 | 129.4 (3) |
C34A—C33—C34B—C35B | −58.6 (11) | C40—Ru1—Ru3—C44 | −5.7 (4) |
C32—C33—C34B—C35B | 43.9 (13) | P1—Ru1—Ru3—C44 | −138.7 (3) |
C33—C34B—C35B—C36B | −51.6 (14) | Ru4—Ru1—Ru3—C44 | −33.0 (3) |
C36A—C31—C36B—C35B | 66.6 (9) | Ru2—Ru1—Ru3—C44 | 34.1 (3) |
C32—C31—C36B—C35B | −47.3 (9) | C41—Ru1—Ru3—C45 | −122.21 (17) |
P2—C31—C36B—C35B | 171.2 (7) | C40—Ru1—Ru3—C45 | 102.6 (3) |
C34B—C35B—C36B—C31 | 55.4 (12) | P1—Ru1—Ru3—C45 | −30.39 (13) |
C6—C1—P1—C13 | 55.3 (3) | Ru4—Ru1—Ru3—C45 | 75.34 (13) |
C2—C1—P1—C13 | −179.0 (3) | Ru2—Ru1—Ru3—C45 | 142.44 (13) |
C6—C1—P1—C7 | 164.9 (3) | C41—Ru1—Ru3—C46 | −19.08 (17) |
C2—C1—P1—C7 | −69.4 (3) | C40—Ru1—Ru3—C46 | −154.2 (3) |
C6—C1—P1—Ru1 | −68.7 (3) | P1—Ru1—Ru3—C46 | 72.74 (13) |
C2—C1—P1—Ru1 | 57.0 (3) | Ru4—Ru1—Ru3—C46 | 178.47 (12) |
C18—C13—P1—C1 | 172.5 (3) | Ru2—Ru1—Ru3—C46 | −114.42 (12) |
C14—C13—P1—C1 | 45.0 (3) | C41—Ru1—Ru3—Ru4 | 162.45 (11) |
C18—C13—P1—C7 | 62.8 (3) | C40—Ru1—Ru3—Ru4 | 27.3 (2) |
C14—C13—P1—C7 | −64.7 (3) | P1—Ru1—Ru3—Ru4 | −105.73 (4) |
C18—C13—P1—Ru1 | −59.4 (3) | Ru2—Ru1—Ru3—Ru4 | 67.11 (2) |
C14—C13—P1—Ru1 | 173.1 (3) | C41—Ru1—Ru3—Ru2 | 95.34 (12) |
C8—C7—P1—C1 | −30.6 (4) | C40—Ru1—Ru3—Ru2 | −39.8 (2) |
C12—C7—P1—C1 | 96.0 (3) | P1—Ru1—Ru3—Ru2 | −172.83 (3) |
C8—C7—P1—C13 | 78.7 (3) | Ru4—Ru1—Ru3—Ru2 | −67.11 (2) |
C12—C7—P1—C13 | −154.7 (3) | O8—C47—Ru4—C49 | 70 (6) |
C8—C7—P1—Ru1 | −160.1 (3) | O8—C47—Ru4—C48 | −23 (6) |
C12—C7—P1—Ru1 | −33.5 (3) | O8—C47—Ru4—Ru3 | −129 (6) |
C30—C25—P2—C19 | −179.2 (3) | O8—C47—Ru4—Ru2 | 167 (6) |
C26—C25—P2—C19 | −49.8 (3) | O8—C47—Ru4—Ru1 | −170 (6) |
C30—C25—P2—C31 | −71.6 (3) | O10—C49—Ru4—C47 | −43 (6) |
C26—C25—P2—C31 | 57.8 (3) | O10—C49—Ru4—C48 | 52 (6) |
C30—C25—P2—Ru2 | 55.6 (3) | O10—C49—Ru4—Ru3 | −146 (5) |
C26—C25—P2—Ru2 | −174.9 (2) | O10—C49—Ru4—Ru2 | −126 (6) |
C24—C19—P2—C25 | −51.2 (3) | O10—C49—Ru4—Ru1 | 170 (6) |
C20—C19—P2—C25 | −175.8 (3) | O9—C48—Ru4—C47 | 58 (3) |
C24—C19—P2—C31 | −159.4 (3) | O9—C48—Ru4—C49 | −37 (3) |
C20—C19—P2—C31 | 76.0 (3) | O9—C48—Ru4—Ru3 | 149 (3) |
C24—C19—P2—Ru2 | 72.0 (3) | O9—C48—Ru4—Ru2 | 131 (3) |
C20—C19—P2—Ru2 | −52.6 (3) | O9—C48—Ru4—Ru1 | −143 (3) |
C36A—C31—P2—C25 | −77.9 (6) | C44—Ru3—Ru4—C47 | 11.46 (16) |
C36B—C31—P2—C25 | −140.9 (5) | C45—Ru3—Ru4—C47 | 102.97 (16) |
C32—C31—P2—C25 | 78.7 (3) | C46—Ru3—Ru4—C47 | −163.1 (8) |
C36A—C31—P2—C19 | 29.3 (6) | Ru2—Ru3—Ru4—C47 | −82.09 (11) |
C36B—C31—P2—C19 | −33.7 (5) | Ru1—Ru3—Ru4—C47 | −153.86 (11) |
C32—C31—P2—C19 | −174.1 (3) | C44—Ru3—Ru4—C49 | 115.3 (4) |
C36A—C31—P2—Ru2 | 157.3 (5) | C45—Ru3—Ru4—C49 | −153.2 (4) |
C36B—C31—P2—Ru2 | 94.3 (5) | C46—Ru3—Ru4—C49 | −59.3 (8) |
C32—C31—P2—Ru2 | −46.1 (4) | Ru2—Ru3—Ru4—C49 | 21.7 (4) |
O2—C41—Ru1—C40 | −159 (7) | Ru1—Ru3—Ru4—C49 | −50.0 (4) |
O2—C41—Ru1—P1 | −66 (7) | C44—Ru3—Ru4—C48 | −82.83 (16) |
O2—C41—Ru1—Ru4 | 79 (7) | C45—Ru3—Ru4—C48 | 8.68 (16) |
O2—C41—Ru1—Ru3 | 44 (7) | C46—Ru3—Ru4—C48 | 102.6 (8) |
O2—C41—Ru1—Ru2 | 104 (7) | Ru2—Ru3—Ru4—C48 | −176.39 (11) |
O1—C40—Ru1—C41 | −146 (4) | Ru1—Ru3—Ru4—C48 | 111.85 (11) |
O1—C40—Ru1—P1 | 127 (4) | C44—Ru3—Ru4—Ru2 | 93.56 (12) |
O1—C40—Ru1—Ru4 | 13 (4) | C45—Ru3—Ru4—Ru2 | −174.94 (11) |
O1—C40—Ru1—Ru3 | −9 (5) | C46—Ru3—Ru4—Ru2 | −81.0 (7) |
O1—C40—Ru1—Ru2 | −43 (4) | Ru1—Ru3—Ru4—Ru2 | −71.76 (2) |
C1—P1—Ru1—C41 | −161.4 (2) | C44—Ru3—Ru4—Ru1 | 165.32 (11) |
C13—P1—Ru1—C41 | 78.30 (19) | C45—Ru3—Ru4—Ru1 | −103.17 (11) |
C7—P1—Ru1—C41 | −39.0 (2) | C46—Ru3—Ru4—Ru1 | −9.3 (7) |
C1—P1—Ru1—C40 | −62.83 (19) | Ru2—Ru3—Ru4—Ru1 | 71.76 (2) |
C13—P1—Ru1—C40 | 176.86 (18) | C43—Ru2—Ru4—C47 | −2.23 (18) |
C7—P1—Ru1—C40 | 59.5 (2) | C42—Ru2—Ru4—C47 | −96.94 (16) |
C1—P1—Ru1—Ru4 | 34.52 (15) | P2—Ru2—Ru4—C47 | 168.5 (2) |
C13—P1—Ru1—Ru4 | −85.78 (14) | Ru3—Ru2—Ru4—C47 | 93.61 (12) |
C7—P1—Ru1—Ru4 | 156.89 (15) | Ru1—Ru2—Ru4—C47 | 164.86 (12) |
C1—P1—Ru1—Ru3 | 93.91 (15) | C43—Ru2—Ru4—C49 | 91.31 (17) |
C13—P1—Ru1—Ru3 | −26.39 (14) | C42—Ru2—Ru4—C49 | −3.39 (16) |
C7—P1—Ru1—Ru3 | −143.72 (15) | P2—Ru2—Ru4—C49 | −98.0 (2) |
C1—P1—Ru1—Ru2 | 67.2 (2) | Ru3—Ru2—Ru4—C49 | −172.85 (12) |
C13—P1—Ru1—Ru2 | −53.1 (2) | Ru1—Ru2—Ru4—C49 | −101.60 (12) |
C7—P1—Ru1—Ru2 | −170.41 (17) | C43—Ru2—Ru4—C48 | −76.2 (6) |
O4—C43—Ru2—C42 | −99 (9) | C42—Ru2—Ru4—C48 | −170.9 (6) |
O4—C43—Ru2—P2 | −3 (9) | P2—Ru2—Ru4—C48 | 94.6 (6) |
O4—C43—Ru2—Ru4 | 175 (100) | Ru3—Ru2—Ru4—C48 | 19.7 (6) |
O4—C43—Ru2—Ru3 | 116 (9) | Ru1—Ru2—Ru4—C48 | 90.9 (6) |
O4—C43—Ru2—Ru1 | 143 (9) | C43—Ru2—Ru4—Ru3 | −95.84 (13) |
O3—C42—Ru2—C43 | −179 (100) | C42—Ru2—Ru4—Ru3 | 169.46 (10) |
O3—C42—Ru2—P2 | 90 (7) | P2—Ru2—Ru4—Ru3 | 74.87 (16) |
O3—C42—Ru2—Ru4 | −79 (7) | Ru1—Ru2—Ru4—Ru3 | 71.253 (17) |
O3—C42—Ru2—Ru3 | −65 (7) | C43—Ru2—Ru4—Ru1 | −167.09 (13) |
O3—C42—Ru2—Ru1 | −18 (7) | C42—Ru2—Ru4—Ru1 | 98.21 (10) |
C25—P2—Ru2—C43 | −164.09 (19) | P2—Ru2—Ru4—Ru1 | 3.62 (16) |
C19—P2—Ru2—C43 | 78.07 (18) | Ru3—Ru2—Ru4—Ru1 | −71.253 (17) |
C31—P2—Ru2—C43 | −43.8 (2) | C41—Ru1—Ru4—C47 | 4.8 (3) |
C25—P2—Ru2—C42 | −68.53 (17) | C40—Ru1—Ru4—C47 | −118.3 (2) |
C19—P2—Ru2—C42 | 173.63 (16) | P1—Ru1—Ru4—C47 | 145.4 (2) |
C31—P2—Ru2—C42 | 51.81 (19) | Ru3—Ru1—Ru4—C47 | 47.34 (19) |
C25—P2—Ru2—Ru4 | 25.1 (2) | Ru2—Ru1—Ru4—C47 | −25.64 (19) |
C19—P2—Ru2—Ru4 | −92.8 (2) | C41—Ru1—Ru4—C49 | 122.3 (3) |
C31—P2—Ru2—Ru4 | 145.4 (2) | C40—Ru1—Ru4—C49 | −0.87 (17) |
C25—P2—Ru2—Ru3 | 93.77 (14) | P1—Ru1—Ru4—C49 | −97.17 (13) |
C19—P2—Ru2—Ru3 | −24.07 (13) | Ru3—Ru1—Ru4—C49 | 164.77 (12) |
C31—P2—Ru2—Ru3 | −145.89 (16) | Ru2—Ru1—Ru4—C49 | 91.80 (12) |
C25—P2—Ru2—Ru1 | 28.40 (14) | C41—Ru1—Ru4—C48 | −138.0 (3) |
C19—P2—Ru2—Ru1 | −89.44 (12) | C40—Ru1—Ru4—C48 | 98.91 (18) |
C31—P2—Ru2—Ru1 | 148.74 (16) | P1—Ru1—Ru4—C48 | 2.61 (15) |
C41—Ru1—Ru2—C43 | −131.5 (4) | Ru3—Ru1—Ru4—C48 | −95.45 (14) |
C40—Ru1—Ru2—C43 | 128.4 (4) | Ru2—Ru1—Ru4—C48 | −168.43 (14) |
P1—Ru1—Ru2—C43 | −1.5 (4) | C41—Ru1—Ru4—Ru3 | −42.5 (3) |
Ru4—Ru1—Ru2—C43 | 35.6 (4) | C40—Ru1—Ru4—Ru3 | −165.64 (11) |
Ru3—Ru1—Ru2—C43 | −31.3 (4) | P1—Ru1—Ru4—Ru3 | 98.06 (4) |
C41—Ru1—Ru2—C42 | 111.06 (17) | Ru2—Ru1—Ru4—Ru3 | −72.980 (19) |
C40—Ru1—Ru2—C42 | 10.93 (16) | C41—Ru1—Ru4—Ru2 | 30.5 (3) |
P1—Ru1—Ru2—C42 | −118.99 (17) | C40—Ru1—Ru4—Ru2 | −92.66 (12) |
Ru4—Ru1—Ru2—C42 | −81.87 (11) | P1—Ru1—Ru4—Ru2 | 171.04 (3) |
Ru3—Ru1—Ru2—C42 | −148.80 (11) | Ru3—Ru1—Ru4—Ru2 | 72.980 (19) |
Experimental details
Crystal data | |
Chemical formula | [Ru4H4(C18H33P)2(CO)10] |
Mr | 1249.24 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 153 |
a, b, c (Å) | 12.461 (5), 23.934 (5), 18.541 (5) |
β (°) | 96.545 (5) |
V (Å3) | 5494 (3) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.19 |
Crystal size (mm) | 0.30 × 0.30 × 0.12 |
Data collection | |
Diffractometer | Stoe & Cie IPDS diffractometer |
Absorption correction | Empirical (using intensity measurements) (Walker & Stuart, 1983) |
Tmin, Tmax | 0.641, 0.895 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 38794, 10053, 6046 |
Rint | 0.057 |
(sin θ/λ)max (Å−1) | 0.615 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.045, 0.75 |
No. of reflections | 10053 |
No. of parameters | 586 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.48, −0.49 |
Computer programs: EXPOSE in IPDS Software (Stoe & Cie, 2000), CELL in IPDS Software, INTEGRATE in IPDS Software, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), ORTEP-3 (Farrugia, 1997), SHELXL97.
P1—Ru1 | 2.3894 (12) | Ru1—Ru2 | 3.0484 (12) |
P2—Ru2 | 2.3824 (11) | Ru2—Ru4 | 2.7977 (6) |
Ru1—Ru4 | 3.0031 (9) | Ru2—Ru3 | 2.9600 (7) |
Ru1—Ru3 | 3.0267 (7) | Ru3—Ru4 | 2.7824 (8) |
P1—Ru1—Ru4 | 113.69 (3) | P2—Ru2—Ru1 | 107.43 (3) |
P1—Ru1—Ru3 | 109.62 (3) | Ru4—Ru2—Ru1 | 61.642 (11) |
Ru4—Ru1—Ru3 | 54.960 (18) | Ru3—Ru2—Ru1 | 60.475 (14) |
P1—Ru1—Ru2 | 166.33 (3) | Ru4—Ru3—Ru2 | 58.216 (12) |
Ru4—Ru1—Ru2 | 55.07 (2) | Ru4—Ru3—Ru1 | 62.088 (18) |
Ru3—Ru1—Ru2 | 58.316 (16) | Ru2—Ru3—Ru1 | 61.21 (2) |
P2—Ru2—Ru4 | 169.05 (3) | Ru3—Ru4—Ru2 | 64.070 (18) |
P2—Ru2—Ru3 | 118.85 (3) | Ru3—Ru4—Ru1 | 62.952 (13) |
Ru4—Ru2—Ru3 | 57.714 (18) | Ru2—Ru4—Ru1 | 63.29 (2) |
It has been shown by Bruce and co-workers that the hydrogenation of Ru3(CO)12 in the presence of tertiary phosphines [L = P(OMe)3, PMe3, PPh3 or PPh(OMe)2)] gives a mixture of tetranuclear complexes [H4Ru4(CO)12-n(L)n] (n = 1–3) (Bruce et al., 1986). From a different starting material, [H2Ru3(CO)6(PCy3)3] (Süss-Fink et al., 1998), but also by hydrogenation in an autoclave, we have obtained the analogous compound [H4Ru4(CO)10(PCy3)2], (I), containing two tricyclohexylphospine (PCy3) ligands. The 1H NMR spectrum displays four non-equivalent hydrides, as opposed to the parent cluster [H4Ru4(CO)10{P(OCH3)3}2], which shows only one hydride resonance (Knox & Kaesz, 1971). The hydride ligands adopt a similar arrangement as that observed for [H4Ru4(CO)10(PH2PCH2CH2PPh2)] (Shapley & Richter, 1977).
The molecular structure of (I) (Fig. 1) was confirmed by single-crystal X-ray analysis. The geometry of (I) consists of an asymmetric Ru4 tetrahedral core, with four long metal–metal distances and two shorter ones. The four hydrido ligands bridged the long Ru—Ru bonds, as suggested for [H4Ru4(CO)10(PPh3)2] (Wilson et al., 1978; Sasvári et al., 1979). The metal–metal distances (long Ru—Ru, average 3.01 Å; short 2.79 Å) are slightly longer from those in [H4Ru4(CO)10(PPh3)2] (long 2.97 Å; short 2.77 Å) and in [H4Ru4(CO)10{P(OMe)3}2] (long 2.973 Å; short 2.792 Å) (Aime et al. 1995). The phosphine ligands are coordinated to Ru1 and Ru2 with Ru—P distances of 2.389 (1) and 2.382 (1) Å, respectively. The P1—Ru1—Ru2—P2 torsion angle is 143.6 (1)°. All the carbonyl groups adopt a staggered conformation with respect to the metal edges. The carbonyl groups opposite to the unbridged Ru—Ru bonds (C46 and C48) show longer Ru—C distances (average 1.913 Å) than those opposite to bridged Ru—Ru bonds (average 1.878 Å). Otherwise no significant difference was observed in the carbonyl envelopes of the three analogous clusters.