metal-organic compounds
[μ-Bis(di-o-tolylphosphanyl)methane-1:2κ2P:P′]decacarbonyl-1κ3C,2κ3C,3κ4C-triangulo-triruthenium(0)–methanol (8/1)
aChemical Sciences Programme, School of Distance Education, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia, and bX-ray Crystallography Unit, School of Physics, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia
*Correspondence e-mail: omarsa@usm.my
The 3(C29H30P2)(CO)10].1/8CH3OH, contains two triangulo-triruthenium molecules with similar configurations and a methanol solvent molecule (fractional site occupancy for the latter = 0.25). The bis(di-o-tolylphosphanyl)methane ligand bridges an Ru—Ru bond and its P atoms are equatorial with respect to the Ru3 triangle. The phosphine-substituted Ru atoms each bear one equatorial and two axial terminal carbonyl ligands whereas the unsubstituted Ru atom carries two equatorial and two axial terminal carbonyl ligands. The dihedral angles between the two benzene rings attached to each P atom are 76.26 (13) and 74.76 (15)° for the first molecule and 77.21 (13) and 75.68 (14)° for the second. In the crystal, molecules are linked into [001] chains via intermolecular C—H⋯O hydrogen bonds. Weak intermolecular C—H⋯π interactions also occur.
of the title compound, [RuRelated literature
For general background to triangulo-triruthenium derivatives, see: Bruce, et al. (1985, 1988a,b). For related structures, see: Shawkataly et al. (1998, 2004, 2010). For the synthesis of bis(di-o-tolylphosphanyl)methane, see: Filby et al. (2006). For the stability of the temperature controller used in the data collection, see: Cosier & Glazer (1986).
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2009); cell SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009).
Supporting information
10.1107/S1600536811000791/hb5784sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536811000791/hb5784Isup2.hkl
All manipulations were performed under a dry oxygen-free nitrogen atmosphere using standard Schlenk techniques. All solvents were dried over sodium and distilled from sodium benzophenone ketyl under dry oxygen free nitrogen. Bis(di-o-tolylphosphanyl)methane (Filby et al., 2006) was prepared by reported procedure. Equimolar quantities of Ru3(CO)12 and bis(di-o-tolylphosphanyl)methane were stirred in THF (25 ml) under nitrogen. About 0.2 ml of diphenylketyl
initiator was introduced into the reaction mixture under a current of nitrogen. The reaction mixture turned intense red. After 10 minutes of stirring the solvent was removed under vacuum. The reaction mixture was separated by TLC (acetone: hexane, 10:90) three bands appeared. The major band (red) was separated and characterized. Orange needles of the title compound were grown by slow solvent / solvent diffusion of CH3OH into CH2Cl2.All hydrogen atoms were positioned geometrically and refined using a riding model with C—H = 0.93–0.97 Å and Uiso(H) = 1.2 or 1.5 Ueq(C). Rotating group model was applied for the methyl group. The solvent molecule is modeled to be a methanol. The occupancy of methanol molecule is fixed to 0.25 and the O–C bond distance is restrained with a distance of 1.50 (1) Å. The methanol solvent is refined isotropically. The maximum and minimum residual electron density peaks of 1.14 and -0.72 e Å-3 were located 0.64 and 0.71 Å from the H40C and Ru2B atoms, respectively.
Data collection: APEX2 (Bruker, 2009); cell
SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).8[Ru3(C29H30P2)(CO)10]·CH4O | F(000) = 4066 |
Mr = 8222.28 | Dx = 1.703 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9981 reflections |
a = 22.7156 (13) Å | θ = 2.5–31.9° |
b = 19.9023 (11) Å | µ = 1.25 mm−1 |
c = 18.4979 (10) Å | T = 100 K |
β = 106.561 (1)° | Needle, orange |
V = 8015.8 (8) Å3 | 0.23 × 0.10 × 0.06 mm |
Z = 1 |
Bruker APEXII DUO CCD diffractometer | 28473 independent reflections |
Radiation source: fine-focus sealed tube | 20091 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.056 |
ϕ and ω scans | θmax = 32.4°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Bruker, 2009) | h = −34→34 |
Tmin = 0.758, Tmax = 0.932 | k = −26→29 |
107136 measured reflections | l = −25→27 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.082 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0264P)2 + 3.1179P] where P = (Fo2 + 2Fc2)/3 |
28473 reflections | (Δ/σ)max = 0.002 |
990 parameters | Δρmax = 1.14 e Å−3 |
1 restraint | Δρmin = −0.72 e Å−3 |
8[Ru3(C29H30P2)(CO)10]·CH4O | V = 8015.8 (8) Å3 |
Mr = 8222.28 | Z = 1 |
Monoclinic, P21/c | Mo Kα radiation |
a = 22.7156 (13) Å | µ = 1.25 mm−1 |
b = 19.9023 (11) Å | T = 100 K |
c = 18.4979 (10) Å | 0.23 × 0.10 × 0.06 mm |
β = 106.561 (1)° |
Bruker APEXII DUO CCD diffractometer | 28473 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2009) | 20091 reflections with I > 2σ(I) |
Tmin = 0.758, Tmax = 0.932 | Rint = 0.056 |
107136 measured reflections |
R[F2 > 2σ(F2)] = 0.035 | 1 restraint |
wR(F2) = 0.082 | H-atom parameters constrained |
S = 1.03 | Δρmax = 1.14 e Å−3 |
28473 reflections | Δρmin = −0.72 e Å−3 |
990 parameters |
Experimental. The crystal was placed in the cold stream of an Oxford Cryosystems Cobra open-flow nitrogen cryostat (Cosier & Glazer, 1986) operating at 100.0 (1) K. |
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) | |
Ru1A | 0.220302 (9) | 0.677332 (10) | 0.085362 (11) | 0.01552 (4) | |
Ru2A | 0.101706 (9) | 0.679317 (10) | 0.107074 (11) | 0.01676 (4) | |
Ru3A | 0.155914 (10) | 0.555256 (11) | 0.087520 (12) | 0.02137 (5) | |
P1A | 0.23685 (3) | 0.79201 (3) | 0.11282 (3) | 0.01575 (12) | |
P2A | 0.09283 (3) | 0.79598 (3) | 0.09101 (3) | 0.01690 (12) | |
O1A | 0.29531 (9) | 0.64003 (11) | 0.24630 (11) | 0.0303 (4) | |
O2A | 0.14958 (9) | 0.70117 (11) | −0.08085 (10) | 0.0286 (4) | |
O3A | 0.33234 (9) | 0.63612 (11) | 0.03704 (11) | 0.0343 (5) | |
O4A | 0.17311 (9) | 0.69638 (10) | 0.27390 (10) | 0.0279 (4) | |
O5A | 0.02466 (9) | 0.66139 (10) | −0.05763 (10) | 0.0276 (4) | |
O6A | −0.01057 (10) | 0.63248 (12) | 0.15217 (12) | 0.0405 (6) | |
O7A | 0.18600 (13) | 0.54704 (12) | 0.25985 (12) | 0.0469 (6) | |
O8A | 0.11455 (10) | 0.55392 (11) | −0.08609 (12) | 0.0376 (5) | |
O9A | 0.26875 (10) | 0.47068 (11) | 0.09090 (13) | 0.0384 (5) | |
O10A | 0.05042 (12) | 0.45816 (14) | 0.07945 (16) | 0.0622 (8) | |
C1A | 0.26433 (11) | 0.84455 (13) | 0.04703 (13) | 0.0186 (5) | |
C2A | 0.27857 (12) | 0.91336 (14) | 0.05881 (15) | 0.0241 (5) | |
C3A | 0.29300 (13) | 0.94867 (15) | 0.00094 (16) | 0.0290 (6) | |
H3AA | 0.3026 | 0.9941 | 0.0078 | 0.035* | |
C4A | 0.29350 (13) | 0.91861 (15) | −0.06618 (16) | 0.0304 (6) | |
H4AA | 0.3021 | 0.9441 | −0.1041 | 0.037* | |
C5A | 0.28134 (12) | 0.85113 (15) | −0.07691 (15) | 0.0261 (6) | |
H5AA | 0.2826 | 0.8303 | −0.1214 | 0.031* | |
C6A | 0.26713 (11) | 0.81470 (13) | −0.02028 (14) | 0.0203 (5) | |
H6AA | 0.2592 | 0.7689 | −0.0273 | 0.024* | |
C7A | 0.28948 (11) | 0.80688 (12) | 0.20754 (13) | 0.0177 (5) | |
C8A | 0.35360 (12) | 0.80422 (13) | 0.22137 (14) | 0.0206 (5) | |
C9A | 0.39014 (13) | 0.81449 (14) | 0.29506 (15) | 0.0270 (6) | |
H9AA | 0.4326 | 0.8136 | 0.3046 | 0.032* | |
C10A | 0.36610 (14) | 0.82584 (14) | 0.35419 (15) | 0.0303 (6) | |
H10A | 0.3920 | 0.8335 | 0.4024 | 0.036* | |
C11A | 0.30257 (14) | 0.82582 (14) | 0.34126 (15) | 0.0277 (6) | |
H11A | 0.2856 | 0.8319 | 0.3810 | 0.033* | |
C12A | 0.26502 (13) | 0.81657 (13) | 0.26826 (14) | 0.0233 (5) | |
H12A | 0.2226 | 0.8168 | 0.2595 | 0.028* | |
C13A | 0.16700 (11) | 0.84055 (13) | 0.11510 (15) | 0.0207 (5) | |
H13A | 0.1742 | 0.8590 | 0.1654 | 0.025* | |
H13B | 0.1630 | 0.8782 | 0.0808 | 0.025* | |
C14A | 0.05547 (11) | 0.82095 (12) | −0.00663 (13) | 0.0184 (5) | |
C15A | −0.00846 (12) | 0.81429 (13) | −0.03756 (14) | 0.0222 (5) | |
C16A | −0.03425 (13) | 0.83291 (14) | −0.11266 (15) | 0.0270 (6) | |
H16A | −0.0766 | 0.8298 | −0.1333 | 0.032* | |
C17A | 0.00073 (14) | 0.85565 (15) | −0.15703 (15) | 0.0307 (6) | |
H17A | −0.0179 | 0.8682 | −0.2067 | 0.037* | |
C18A | 0.06415 (14) | 0.85982 (15) | −0.12748 (16) | 0.0305 (6) | |
H18A | 0.0883 | 0.8739 | −0.1576 | 0.037* | |
C19A | 0.09110 (12) | 0.84276 (14) | −0.05254 (15) | 0.0232 (5) | |
H19A | 0.1335 | 0.8459 | −0.0326 | 0.028* | |
C20A | 0.05500 (12) | 0.84311 (14) | 0.15128 (14) | 0.0238 (5) | |
C21A | 0.03789 (15) | 0.91107 (17) | 0.14213 (18) | 0.0368 (7) | |
C22A | 0.01195 (18) | 0.9402 (2) | 0.1944 (2) | 0.0509 (10) | |
H22A | −0.0012 | 0.9846 | 0.1876 | 0.061* | |
C23A | 0.00516 (15) | 0.9050 (2) | 0.25650 (19) | 0.0448 (9) | |
H23A | −0.0118 | 0.9260 | 0.2908 | 0.054* | |
C24A | 0.02358 (14) | 0.83938 (18) | 0.26684 (17) | 0.0363 (7) | |
H24A | 0.0201 | 0.8156 | 0.3087 | 0.044* | |
C25A | 0.04761 (12) | 0.80862 (16) | 0.21368 (14) | 0.0259 (6) | |
H25A | 0.0591 | 0.7637 | 0.2201 | 0.031* | |
C26A | 0.28218 (14) | 0.95086 (14) | 0.13111 (16) | 0.0302 (6) | |
H26A | 0.2807 | 0.9983 | 0.1216 | 0.045* | |
H26B | 0.3200 | 0.9399 | 0.1683 | 0.045* | |
H26C | 0.2482 | 0.9382 | 0.1493 | 0.045* | |
C27A | 0.38495 (13) | 0.79109 (16) | 0.16094 (16) | 0.0309 (6) | |
H27A | 0.4269 | 0.7783 | 0.1841 | 0.046* | |
H27B | 0.3839 | 0.8311 | 0.1316 | 0.046* | |
H27C | 0.3641 | 0.7555 | 0.1287 | 0.046* | |
C28A | −0.05019 (12) | 0.78985 (16) | 0.00726 (16) | 0.0307 (6) | |
H28A | −0.0865 | 0.7706 | −0.0263 | 0.046* | |
H28B | −0.0614 | 0.8269 | 0.0338 | 0.046* | |
H28C | −0.0292 | 0.7565 | 0.0428 | 0.046* | |
C29A | 0.0455 (2) | 0.95446 (19) | 0.0783 (2) | 0.0667 (14) | |
H29A | 0.0342 | 0.9999 | 0.0855 | 0.100* | |
H29B | 0.0195 | 0.9378 | 0.0312 | 0.100* | |
H29C | 0.0875 | 0.9532 | 0.0774 | 0.100* | |
C30A | 0.26436 (12) | 0.65347 (13) | 0.18781 (15) | 0.0217 (5) | |
C31A | 0.17239 (12) | 0.69159 (13) | −0.01808 (15) | 0.0215 (5) | |
C32A | 0.29057 (12) | 0.65169 (14) | 0.05549 (14) | 0.0225 (5) | |
C33A | 0.14982 (12) | 0.68880 (13) | 0.21078 (15) | 0.0216 (5) | |
C34A | 0.05662 (12) | 0.66612 (13) | 0.00228 (15) | 0.0220 (5) | |
C35A | 0.03166 (13) | 0.65093 (15) | 0.13479 (15) | 0.0256 (6) | |
C36A | 0.17545 (15) | 0.55492 (15) | 0.19671 (17) | 0.0324 (6) | |
C37A | 0.13004 (13) | 0.55914 (14) | −0.02258 (16) | 0.0268 (6) | |
C38A | 0.22584 (14) | 0.50192 (14) | 0.08860 (16) | 0.0277 (6) | |
C39A | 0.08977 (15) | 0.49406 (16) | 0.08308 (19) | 0.0377 (7) | |
Ru1B | 0.282548 (9) | 0.326339 (10) | 0.936357 (11) | 0.01576 (4) | |
Ru2B | 0.399429 (9) | 0.309121 (10) | 0.911319 (11) | 0.01557 (4) | |
Ru3B | 0.354149 (10) | 0.440860 (10) | 0.922137 (12) | 0.02002 (5) | |
P1B | 0.25992 (3) | 0.21187 (3) | 0.91452 (3) | 0.01521 (12) | |
P2B | 0.40317 (3) | 0.19375 (3) | 0.93823 (3) | 0.01592 (12) | |
O1B | 0.21008 (10) | 0.36087 (11) | 0.77383 (11) | 0.0333 (5) | |
O2B | 0.35113 (9) | 0.30992 (10) | 1.10464 (10) | 0.0276 (4) | |
O3B | 0.17110 (9) | 0.37604 (11) | 0.98056 (11) | 0.0341 (5) | |
O4B | 0.32795 (9) | 0.28896 (10) | 0.74471 (10) | 0.0260 (4) | |
O5B | 0.47536 (9) | 0.33369 (10) | 1.07514 (10) | 0.0254 (4) | |
O6B | 0.51458 (9) | 0.34127 (12) | 0.86489 (12) | 0.0348 (5) | |
O7B | 0.32373 (13) | 0.43605 (11) | 0.74972 (12) | 0.0489 (7) | |
O8B | 0.39854 (10) | 0.45298 (11) | 1.09512 (11) | 0.0333 (5) | |
O9B | 0.24943 (10) | 0.53881 (11) | 0.91616 (14) | 0.0419 (6) | |
O10B | 0.46223 (11) | 0.52956 (13) | 0.91726 (16) | 0.0551 (7) | |
C1B | 0.22076 (11) | 0.19372 (12) | 0.81543 (13) | 0.0179 (5) | |
C2B | 0.15836 (11) | 0.20918 (13) | 0.78421 (14) | 0.0204 (5) | |
C3B | 0.13122 (13) | 0.19456 (14) | 0.70791 (15) | 0.0249 (6) | |
H3BA | 0.0896 | 0.2031 | 0.6869 | 0.030* | |
C4B | 0.16457 (15) | 0.16782 (15) | 0.66293 (16) | 0.0312 (7) | |
H4BA | 0.1454 | 0.1586 | 0.6124 | 0.037* | |
C5B | 0.22658 (14) | 0.15480 (15) | 0.69321 (15) | 0.0283 (6) | |
H5BA | 0.2495 | 0.1377 | 0.6630 | 0.034* | |
C6B | 0.25418 (12) | 0.16751 (13) | 0.76907 (15) | 0.0225 (5) | |
H6BA | 0.2958 | 0.1584 | 0.7895 | 0.027* | |
C7B | 0.21822 (11) | 0.16697 (12) | 0.97280 (13) | 0.0176 (5) | |
C8B | 0.19090 (12) | 0.10265 (13) | 0.95663 (14) | 0.0212 (5) | |
C9B | 0.17052 (13) | 0.07180 (14) | 1.01206 (16) | 0.0274 (6) | |
H9BA | 0.1519 | 0.0299 | 1.0019 | 0.033* | |
C10B | 0.17656 (13) | 0.10076 (15) | 1.08253 (16) | 0.0286 (6) | |
H10B | 0.1630 | 0.0781 | 1.1187 | 0.034* | |
C11B | 0.20303 (12) | 0.16365 (14) | 1.09782 (15) | 0.0243 (5) | |
H11B | 0.2076 | 0.1837 | 1.1445 | 0.029* | |
C12B | 0.22272 (11) | 0.19645 (13) | 1.04266 (14) | 0.0196 (5) | |
H12B | 0.2394 | 0.2393 | 1.0525 | 0.023* | |
C13B | 0.32775 (11) | 0.15592 (13) | 0.93696 (15) | 0.0206 (5) | |
H13C | 0.3194 | 0.1196 | 0.9005 | 0.025* | |
H13D | 0.3319 | 0.1362 | 0.9861 | 0.025* | |
C14B | 0.42883 (11) | 0.13463 (13) | 0.87695 (14) | 0.0202 (5) | |
C15B | 0.43712 (12) | 0.06521 (14) | 0.89234 (15) | 0.0250 (5) | |
C16B | 0.45645 (15) | 0.02591 (15) | 0.84122 (17) | 0.0347 (7) | |
H16B | 0.4628 | −0.0198 | 0.8509 | 0.042* | |
C17B | 0.46658 (17) | 0.05181 (17) | 0.77716 (18) | 0.0422 (8) | |
H17B | 0.4794 | 0.0238 | 0.7443 | 0.051* | |
C18B | 0.45770 (15) | 0.11917 (16) | 0.76151 (16) | 0.0339 (7) | |
H18B | 0.4637 | 0.1369 | 0.7176 | 0.041* | |
C19B | 0.43979 (12) | 0.16037 (14) | 0.81156 (14) | 0.0242 (5) | |
H19B | 0.4349 | 0.2062 | 0.8016 | 0.029* | |
C20B | 0.45181 (11) | 0.17630 (12) | 1.03454 (13) | 0.0176 (5) | |
C21B | 0.51592 (12) | 0.17446 (13) | 1.05094 (14) | 0.0200 (5) | |
C22B | 0.55078 (13) | 0.16466 (13) | 1.12575 (15) | 0.0245 (6) | |
H22B | 0.5933 | 0.1626 | 1.1367 | 0.029* | |
C23B | 0.52438 (14) | 0.15791 (14) | 1.18371 (16) | 0.0293 (6) | |
H23B | 0.5488 | 0.1512 | 1.2329 | 0.035* | |
C24B | 0.46091 (15) | 0.16130 (15) | 1.16792 (15) | 0.0303 (6) | |
H24B | 0.4425 | 0.1574 | 1.2066 | 0.036* | |
C25B | 0.42512 (13) | 0.17053 (14) | 1.09421 (15) | 0.0242 (5) | |
H25B | 0.3826 | 0.1729 | 1.0840 | 0.029* | |
C26B | 0.11899 (12) | 0.23870 (15) | 0.82941 (15) | 0.0276 (6) | |
H26D | 0.0837 | 0.2600 | 0.7960 | 0.041* | |
H26E | 0.1423 | 0.2713 | 0.8642 | 0.041* | |
H26F | 0.1059 | 0.2036 | 0.8569 | 0.041* | |
C27B | 0.18306 (14) | 0.06476 (14) | 0.88355 (15) | 0.0279 (6) | |
H27D | 0.1715 | 0.0192 | 0.8896 | 0.042* | |
H27E | 0.2211 | 0.0652 | 0.8706 | 0.042* | |
H27F | 0.1516 | 0.0859 | 0.8441 | 0.042* | |
C28B | 0.42639 (13) | 0.03133 (14) | 0.96078 (16) | 0.0283 (6) | |
H28D | 0.4298 | −0.0165 | 0.9563 | 0.042* | |
H28E | 0.3861 | 0.0424 | 0.9640 | 0.042* | |
H28F | 0.4565 | 0.0466 | 1.0055 | 0.042* | |
C29B | 0.55012 (12) | 0.18341 (15) | 0.99213 (15) | 0.0257 (6) | |
H29D | 0.5913 | 0.1980 | 1.0162 | 0.039* | |
H29E | 0.5295 | 0.2165 | 0.9559 | 0.039* | |
H29F | 0.5512 | 0.1414 | 0.9670 | 0.039* | |
C30B | 0.24043 (12) | 0.34815 (13) | 0.83281 (15) | 0.0225 (5) | |
C31B | 0.32887 (11) | 0.31609 (13) | 1.04120 (14) | 0.0200 (5) | |
C32B | 0.21339 (12) | 0.35807 (14) | 0.96398 (14) | 0.0225 (5) | |
C33B | 0.35150 (12) | 0.29737 (13) | 0.80760 (15) | 0.0207 (5) | |
C34B | 0.44434 (11) | 0.32671 (12) | 1.01505 (14) | 0.0188 (5) | |
C35B | 0.47147 (12) | 0.32800 (14) | 0.88280 (15) | 0.0229 (5) | |
C36B | 0.33376 (15) | 0.43294 (14) | 0.81318 (17) | 0.0324 (7) | |
C37B | 0.38139 (12) | 0.44392 (14) | 1.03222 (16) | 0.0247 (5) | |
C38B | 0.28929 (13) | 0.50278 (14) | 0.91896 (16) | 0.0274 (6) | |
C39B | 0.42278 (14) | 0.49617 (15) | 0.91889 (18) | 0.0324 (7) | |
O11 | 0.1574 (5) | 0.9239 (5) | 0.2700 (6) | 0.048 (2)* | 0.25 |
H11O | 0.1805 | 0.9126 | 0.3109 | 0.072* | 0.25 |
C40 | 0.1575 (7) | 0.9966 (5) | 0.2638 (8) | 0.045 (3)* | 0.25 |
H40A | 0.1651 | 1.0163 | 0.3130 | 0.067* | 0.25 |
H40B | 0.1184 | 1.0115 | 0.2324 | 0.067* | 0.25 |
H40C | 0.1892 | 1.0102 | 0.2418 | 0.067* | 0.25 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ru1A | 0.01660 (9) | 0.01669 (9) | 0.01359 (9) | −0.00121 (7) | 0.00484 (7) | −0.00157 (7) |
Ru2A | 0.01694 (9) | 0.01977 (10) | 0.01422 (9) | −0.00106 (7) | 0.00547 (7) | 0.00060 (7) |
Ru3A | 0.02564 (11) | 0.01627 (10) | 0.02350 (11) | −0.00219 (8) | 0.00913 (9) | 0.00056 (8) |
P1A | 0.0161 (3) | 0.0175 (3) | 0.0128 (3) | −0.0016 (2) | 0.0028 (2) | −0.0018 (2) |
P2A | 0.0163 (3) | 0.0210 (3) | 0.0134 (3) | 0.0013 (2) | 0.0041 (2) | −0.0005 (2) |
O1A | 0.0313 (11) | 0.0381 (12) | 0.0194 (10) | 0.0038 (9) | 0.0041 (8) | 0.0050 (9) |
O2A | 0.0283 (11) | 0.0374 (12) | 0.0171 (9) | −0.0088 (9) | 0.0016 (8) | 0.0012 (8) |
O3A | 0.0257 (11) | 0.0491 (14) | 0.0309 (11) | 0.0043 (9) | 0.0124 (9) | −0.0054 (10) |
O4A | 0.0268 (10) | 0.0366 (12) | 0.0189 (10) | 0.0024 (8) | 0.0042 (8) | 0.0006 (8) |
O5A | 0.0289 (10) | 0.0339 (11) | 0.0176 (9) | −0.0050 (8) | 0.0028 (8) | −0.0040 (8) |
O6A | 0.0332 (12) | 0.0565 (16) | 0.0381 (13) | −0.0153 (10) | 0.0203 (10) | −0.0029 (11) |
O7A | 0.0771 (19) | 0.0372 (13) | 0.0275 (12) | −0.0025 (12) | 0.0167 (12) | 0.0075 (10) |
O8A | 0.0439 (13) | 0.0367 (13) | 0.0293 (12) | −0.0007 (10) | 0.0058 (10) | −0.0047 (9) |
O9A | 0.0382 (13) | 0.0356 (13) | 0.0440 (13) | 0.0092 (10) | 0.0159 (11) | 0.0035 (10) |
O10A | 0.0492 (16) | 0.0561 (18) | 0.082 (2) | −0.0274 (13) | 0.0199 (15) | 0.0083 (15) |
C1A | 0.0186 (12) | 0.0211 (12) | 0.0144 (11) | −0.0026 (9) | 0.0022 (9) | 0.0028 (9) |
C2A | 0.0245 (13) | 0.0222 (13) | 0.0217 (13) | −0.0034 (10) | 0.0001 (10) | 0.0021 (10) |
C3A | 0.0337 (15) | 0.0223 (14) | 0.0295 (15) | −0.0058 (11) | 0.0064 (12) | 0.0046 (11) |
C4A | 0.0279 (15) | 0.0358 (17) | 0.0261 (15) | −0.0070 (12) | 0.0054 (12) | 0.0109 (12) |
C5A | 0.0242 (13) | 0.0372 (16) | 0.0163 (12) | −0.0062 (11) | 0.0049 (10) | 0.0019 (11) |
C6A | 0.0193 (12) | 0.0236 (13) | 0.0164 (12) | −0.0054 (10) | 0.0026 (9) | −0.0013 (10) |
C7A | 0.0212 (12) | 0.0167 (11) | 0.0146 (11) | −0.0014 (9) | 0.0042 (9) | −0.0023 (9) |
C8A | 0.0196 (12) | 0.0216 (12) | 0.0184 (12) | 0.0006 (10) | 0.0019 (10) | −0.0014 (10) |
C9A | 0.0223 (13) | 0.0299 (15) | 0.0225 (14) | 0.0002 (11) | −0.0039 (10) | −0.0004 (11) |
C10A | 0.0398 (17) | 0.0275 (15) | 0.0157 (13) | −0.0007 (12) | −0.0049 (11) | −0.0009 (11) |
C11A | 0.0411 (17) | 0.0258 (14) | 0.0163 (13) | −0.0008 (12) | 0.0085 (12) | −0.0017 (10) |
C12A | 0.0301 (14) | 0.0233 (14) | 0.0170 (12) | −0.0017 (11) | 0.0074 (10) | −0.0014 (10) |
C13A | 0.0177 (12) | 0.0192 (12) | 0.0225 (13) | 0.0003 (9) | 0.0014 (10) | −0.0020 (10) |
C14A | 0.0191 (11) | 0.0204 (12) | 0.0144 (11) | 0.0028 (9) | 0.0028 (9) | 0.0001 (9) |
C15A | 0.0211 (12) | 0.0255 (14) | 0.0189 (12) | 0.0032 (10) | 0.0038 (10) | 0.0022 (10) |
C16A | 0.0248 (14) | 0.0318 (15) | 0.0202 (13) | 0.0042 (11) | −0.0002 (10) | −0.0010 (11) |
C17A | 0.0393 (17) | 0.0338 (16) | 0.0166 (13) | 0.0105 (13) | 0.0040 (12) | 0.0036 (11) |
C18A | 0.0392 (17) | 0.0330 (16) | 0.0238 (14) | 0.0058 (13) | 0.0163 (13) | 0.0064 (12) |
C19A | 0.0238 (13) | 0.0266 (14) | 0.0202 (13) | 0.0022 (10) | 0.0075 (10) | 0.0032 (10) |
C20A | 0.0205 (12) | 0.0319 (15) | 0.0190 (13) | 0.0038 (10) | 0.0055 (10) | −0.0075 (11) |
C21A | 0.0435 (19) | 0.0370 (18) | 0.0323 (17) | 0.0137 (14) | 0.0145 (14) | −0.0036 (13) |
C22A | 0.059 (2) | 0.046 (2) | 0.049 (2) | 0.0193 (18) | 0.0177 (19) | −0.0128 (17) |
C23A | 0.0389 (19) | 0.063 (2) | 0.0369 (19) | 0.0066 (16) | 0.0172 (15) | −0.0217 (17) |
C24A | 0.0305 (16) | 0.059 (2) | 0.0217 (15) | −0.0043 (14) | 0.0117 (12) | −0.0141 (14) |
C25A | 0.0169 (12) | 0.0422 (17) | 0.0185 (13) | −0.0017 (11) | 0.0049 (10) | −0.0059 (11) |
C26A | 0.0384 (17) | 0.0213 (14) | 0.0291 (15) | −0.0058 (12) | 0.0066 (13) | −0.0044 (11) |
C27A | 0.0192 (13) | 0.0432 (18) | 0.0289 (15) | 0.0019 (12) | 0.0047 (11) | −0.0063 (13) |
C28A | 0.0187 (13) | 0.0449 (18) | 0.0266 (15) | 0.0008 (12) | 0.0035 (11) | 0.0111 (13) |
C29A | 0.123 (4) | 0.034 (2) | 0.048 (2) | 0.036 (2) | 0.032 (2) | 0.0086 (17) |
C30A | 0.0247 (13) | 0.0215 (13) | 0.0209 (13) | 0.0000 (10) | 0.0093 (10) | −0.0010 (10) |
C31A | 0.0203 (12) | 0.0208 (13) | 0.0245 (13) | −0.0056 (10) | 0.0083 (10) | −0.0038 (10) |
C32A | 0.0261 (13) | 0.0257 (14) | 0.0163 (12) | 0.0010 (10) | 0.0069 (10) | −0.0020 (10) |
C33A | 0.0186 (12) | 0.0238 (13) | 0.0231 (13) | 0.0005 (10) | 0.0072 (10) | 0.0030 (10) |
C34A | 0.0229 (13) | 0.0213 (13) | 0.0229 (13) | −0.0040 (10) | 0.0084 (10) | −0.0003 (10) |
C35A | 0.0272 (14) | 0.0311 (15) | 0.0172 (13) | −0.0017 (11) | 0.0042 (11) | −0.0001 (11) |
C36A | 0.0451 (18) | 0.0233 (15) | 0.0306 (16) | −0.0041 (13) | 0.0139 (14) | 0.0027 (12) |
C37A | 0.0267 (14) | 0.0233 (14) | 0.0300 (15) | −0.0001 (11) | 0.0074 (12) | −0.0021 (11) |
C38A | 0.0369 (16) | 0.0233 (14) | 0.0245 (14) | −0.0017 (12) | 0.0112 (12) | 0.0000 (11) |
C39A | 0.0377 (18) | 0.0317 (17) | 0.0440 (19) | −0.0095 (13) | 0.0120 (15) | 0.0040 (14) |
Ru1B | 0.01691 (9) | 0.01596 (9) | 0.01461 (9) | −0.00020 (7) | 0.00479 (7) | −0.00098 (7) |
Ru2B | 0.01516 (9) | 0.01599 (9) | 0.01511 (9) | 0.00012 (7) | 0.00360 (7) | 0.00120 (7) |
Ru3B | 0.02252 (10) | 0.01495 (10) | 0.02291 (10) | −0.00039 (8) | 0.00702 (8) | 0.00141 (8) |
P1B | 0.0145 (3) | 0.0167 (3) | 0.0140 (3) | −0.0004 (2) | 0.0035 (2) | −0.0006 (2) |
P2B | 0.0142 (3) | 0.0167 (3) | 0.0160 (3) | 0.0008 (2) | 0.0029 (2) | 0.0012 (2) |
O1B | 0.0390 (12) | 0.0398 (13) | 0.0188 (10) | 0.0066 (10) | 0.0046 (9) | 0.0031 (9) |
O2B | 0.0253 (10) | 0.0347 (11) | 0.0209 (10) | −0.0059 (8) | 0.0034 (8) | 0.0001 (8) |
O3B | 0.0278 (11) | 0.0435 (13) | 0.0329 (11) | 0.0073 (9) | 0.0118 (9) | −0.0070 (10) |
O4B | 0.0276 (10) | 0.0290 (11) | 0.0191 (9) | 0.0013 (8) | 0.0028 (8) | −0.0003 (8) |
O5B | 0.0245 (10) | 0.0255 (10) | 0.0221 (10) | 0.0000 (8) | 0.0001 (8) | −0.0010 (8) |
O6B | 0.0268 (11) | 0.0484 (14) | 0.0329 (12) | −0.0059 (9) | 0.0148 (9) | 0.0011 (10) |
O7B | 0.088 (2) | 0.0315 (13) | 0.0271 (12) | −0.0007 (12) | 0.0163 (12) | 0.0076 (10) |
O8B | 0.0356 (12) | 0.0347 (12) | 0.0275 (11) | 0.0008 (9) | 0.0058 (9) | −0.0039 (9) |
O9B | 0.0365 (13) | 0.0320 (12) | 0.0586 (15) | 0.0115 (10) | 0.0156 (11) | 0.0031 (11) |
O10B | 0.0368 (14) | 0.0525 (16) | 0.0769 (19) | −0.0138 (12) | 0.0176 (13) | 0.0188 (14) |
C1B | 0.0213 (12) | 0.0166 (11) | 0.0154 (11) | −0.0029 (9) | 0.0049 (9) | −0.0011 (9) |
C2B | 0.0185 (12) | 0.0221 (13) | 0.0193 (12) | −0.0027 (9) | 0.0036 (10) | 0.0010 (10) |
C3B | 0.0230 (13) | 0.0291 (14) | 0.0189 (13) | −0.0050 (11) | −0.0001 (10) | 0.0030 (11) |
C4B | 0.0442 (18) | 0.0309 (16) | 0.0175 (13) | −0.0134 (13) | 0.0069 (12) | −0.0043 (11) |
C5B | 0.0384 (16) | 0.0294 (15) | 0.0216 (14) | −0.0102 (12) | 0.0156 (12) | −0.0082 (11) |
C6B | 0.0242 (13) | 0.0217 (13) | 0.0240 (13) | −0.0030 (10) | 0.0106 (11) | −0.0037 (10) |
C7B | 0.0173 (11) | 0.0194 (12) | 0.0155 (11) | 0.0005 (9) | 0.0037 (9) | 0.0024 (9) |
C8B | 0.0216 (12) | 0.0197 (12) | 0.0216 (13) | 0.0008 (10) | 0.0050 (10) | 0.0011 (10) |
C9B | 0.0322 (15) | 0.0224 (14) | 0.0304 (15) | −0.0030 (11) | 0.0134 (12) | 0.0021 (11) |
C10B | 0.0335 (15) | 0.0291 (15) | 0.0263 (14) | 0.0029 (12) | 0.0135 (12) | 0.0097 (12) |
C11B | 0.0230 (13) | 0.0313 (15) | 0.0185 (13) | 0.0029 (11) | 0.0061 (10) | 0.0020 (11) |
C12B | 0.0169 (11) | 0.0226 (12) | 0.0184 (12) | −0.0005 (9) | 0.0038 (9) | 0.0011 (10) |
C13B | 0.0163 (11) | 0.0178 (12) | 0.0252 (13) | 0.0005 (9) | 0.0020 (10) | 0.0033 (10) |
C14B | 0.0188 (12) | 0.0202 (12) | 0.0187 (12) | 0.0015 (9) | 0.0008 (9) | −0.0024 (10) |
C15B | 0.0251 (13) | 0.0210 (13) | 0.0259 (14) | 0.0026 (10) | 0.0024 (11) | −0.0018 (11) |
C16B | 0.0465 (19) | 0.0236 (15) | 0.0312 (16) | 0.0081 (13) | 0.0067 (14) | −0.0057 (12) |
C17B | 0.059 (2) | 0.0371 (19) | 0.0301 (17) | 0.0154 (16) | 0.0111 (15) | −0.0125 (14) |
C18B | 0.0442 (18) | 0.0375 (18) | 0.0184 (14) | 0.0064 (14) | 0.0066 (13) | −0.0039 (12) |
C19B | 0.0256 (14) | 0.0267 (14) | 0.0194 (13) | 0.0032 (11) | 0.0051 (10) | −0.0010 (10) |
C20B | 0.0200 (12) | 0.0163 (11) | 0.0161 (11) | 0.0011 (9) | 0.0046 (9) | 0.0014 (9) |
C21B | 0.0211 (12) | 0.0178 (12) | 0.0196 (12) | 0.0010 (9) | 0.0035 (10) | 0.0010 (10) |
C22B | 0.0229 (13) | 0.0224 (13) | 0.0227 (13) | 0.0021 (10) | −0.0024 (10) | −0.0002 (10) |
C23B | 0.0380 (17) | 0.0267 (15) | 0.0188 (13) | 0.0042 (12) | 0.0007 (12) | 0.0003 (11) |
C24B | 0.0443 (18) | 0.0322 (16) | 0.0167 (13) | 0.0041 (13) | 0.0127 (12) | 0.0018 (11) |
C25B | 0.0256 (13) | 0.0245 (14) | 0.0237 (13) | 0.0035 (10) | 0.0088 (11) | 0.0018 (11) |
C26B | 0.0192 (13) | 0.0375 (16) | 0.0233 (14) | 0.0043 (11) | 0.0017 (11) | −0.0020 (12) |
C27B | 0.0394 (16) | 0.0201 (13) | 0.0252 (14) | −0.0091 (11) | 0.0105 (12) | −0.0038 (11) |
C28B | 0.0269 (14) | 0.0195 (13) | 0.0397 (17) | 0.0025 (11) | 0.0115 (12) | 0.0036 (12) |
C29B | 0.0170 (12) | 0.0331 (16) | 0.0260 (14) | 0.0019 (11) | 0.0043 (10) | 0.0028 (11) |
C30B | 0.0267 (13) | 0.0199 (13) | 0.0229 (13) | 0.0008 (10) | 0.0104 (11) | −0.0024 (10) |
C31B | 0.0194 (12) | 0.0192 (12) | 0.0217 (13) | −0.0048 (9) | 0.0063 (10) | −0.0029 (10) |
C32B | 0.0245 (13) | 0.0252 (14) | 0.0177 (12) | −0.0019 (10) | 0.0058 (10) | −0.0035 (10) |
C33B | 0.0196 (12) | 0.0193 (12) | 0.0233 (13) | 0.0015 (9) | 0.0060 (10) | 0.0038 (10) |
C34B | 0.0175 (11) | 0.0167 (12) | 0.0220 (13) | −0.0012 (9) | 0.0056 (10) | 0.0002 (10) |
C35B | 0.0213 (12) | 0.0255 (13) | 0.0199 (13) | −0.0013 (10) | 0.0027 (10) | 0.0012 (10) |
C36B | 0.0477 (19) | 0.0186 (14) | 0.0315 (16) | −0.0011 (12) | 0.0124 (14) | 0.0040 (12) |
C37B | 0.0250 (13) | 0.0214 (13) | 0.0284 (14) | 0.0014 (10) | 0.0089 (11) | 0.0001 (11) |
C38B | 0.0308 (15) | 0.0212 (14) | 0.0303 (15) | −0.0018 (11) | 0.0090 (12) | 0.0010 (11) |
C39B | 0.0264 (15) | 0.0307 (16) | 0.0398 (17) | −0.0023 (12) | 0.0090 (13) | 0.0072 (13) |
Ru1A—C32A | 1.902 (3) | Ru1B—P1B | 2.3450 (7) |
Ru1A—C30A | 1.933 (3) | Ru1B—Ru2B | 2.8429 (3) |
Ru1A—C31A | 1.934 (3) | Ru1B—Ru3B | 2.8554 (3) |
Ru1A—P1A | 2.3451 (7) | Ru2B—C35B | 1.895 (3) |
Ru1A—Ru2A | 2.8350 (3) | Ru2B—C34B | 1.931 (3) |
Ru1A—Ru3A | 2.8420 (3) | Ru2B—C33B | 1.931 (3) |
Ru2A—C35A | 1.892 (3) | Ru2B—P2B | 2.3459 (7) |
Ru2A—C33A | 1.927 (3) | Ru2B—Ru3B | 2.8442 (3) |
Ru2A—C34A | 1.935 (3) | Ru3B—C38B | 1.909 (3) |
Ru2A—P2A | 2.3422 (7) | Ru3B—C39B | 1.923 (3) |
Ru2A—Ru3A | 2.8280 (3) | Ru3B—C36B | 1.941 (3) |
Ru3A—C38A | 1.906 (3) | Ru3B—C37B | 1.953 (3) |
Ru3A—C39A | 1.918 (3) | P1B—C1B | 1.831 (2) |
Ru3A—C36A | 1.940 (3) | P1B—C13B | 1.850 (2) |
Ru3A—C37A | 1.954 (3) | P1B—C7B | 1.855 (2) |
P1A—C7A | 1.842 (2) | P2B—C14B | 1.840 (3) |
P1A—C1A | 1.843 (2) | P2B—C20B | 1.842 (2) |
P1A—C13A | 1.869 (3) | P2B—C13B | 1.865 (3) |
P2A—C14A | 1.832 (2) | O1B—C30B | 1.141 (3) |
P2A—C13A | 1.843 (3) | O2B—C31B | 1.144 (3) |
P2A—C20A | 1.846 (3) | O3B—C32B | 1.146 (3) |
O1A—C30A | 1.141 (3) | O4B—C33B | 1.146 (3) |
O2A—C31A | 1.145 (3) | O5B—C34B | 1.142 (3) |
O3A—C32A | 1.139 (3) | O6B—C35B | 1.150 (3) |
O4A—C33A | 1.146 (3) | O7B—C36B | 1.132 (3) |
O5A—C34A | 1.143 (3) | O8B—C37B | 1.131 (3) |
O6A—C35A | 1.155 (3) | O9B—C38B | 1.145 (3) |
O7A—C36A | 1.134 (3) | O10B—C39B | 1.123 (3) |
O8A—C37A | 1.131 (3) | C1B—C6B | 1.398 (3) |
O9A—C38A | 1.147 (3) | C1B—C2B | 1.404 (3) |
O10A—C39A | 1.131 (4) | C2B—C3B | 1.400 (4) |
C1A—C6A | 1.397 (3) | C2B—C26B | 1.507 (4) |
C1A—C2A | 1.410 (4) | C3B—C4B | 1.381 (4) |
C2A—C3A | 1.395 (4) | C3B—H3BA | 0.9300 |
C2A—C26A | 1.513 (4) | C4B—C5B | 1.384 (4) |
C3A—C4A | 1.381 (4) | C4B—H4BA | 0.9300 |
C3A—H3AA | 0.9300 | C5B—C6B | 1.387 (4) |
C4A—C5A | 1.374 (4) | C5B—H5BA | 0.9300 |
C4A—H4AA | 0.9300 | C6B—H6BA | 0.9300 |
C5A—C6A | 1.386 (3) | C7B—C12B | 1.396 (3) |
C5A—H5AA | 0.9300 | C7B—C8B | 1.417 (3) |
C6A—H6AA | 0.9300 | C8B—C9B | 1.383 (4) |
C7A—C12A | 1.401 (3) | C8B—C27B | 1.513 (4) |
C7A—C8A | 1.406 (3) | C9B—C10B | 1.396 (4) |
C8A—C9A | 1.394 (3) | C9B—H9BA | 0.9300 |
C8A—C27A | 1.510 (4) | C10B—C11B | 1.382 (4) |
C9A—C10A | 1.373 (4) | C10B—H10B | 0.9300 |
C9A—H9AA | 0.9300 | C11B—C12B | 1.388 (3) |
C10A—C11A | 1.394 (4) | C11B—H11B | 0.9300 |
C10A—H10A | 0.9300 | C12B—H12B | 0.9300 |
C11A—C12A | 1.389 (4) | C13B—H13C | 0.9700 |
C11A—H11A | 0.9300 | C13B—H13D | 0.9700 |
C12A—H12A | 0.9300 | C14B—C19B | 1.400 (4) |
C13A—H13A | 0.9700 | C14B—C15B | 1.412 (4) |
C13A—H13B | 0.9700 | C15B—C16B | 1.391 (4) |
C14A—C19A | 1.399 (3) | C15B—C28B | 1.514 (4) |
C14A—C15A | 1.407 (3) | C16B—C17B | 1.370 (4) |
C15A—C16A | 1.395 (4) | C16B—H16B | 0.9300 |
C15A—C28A | 1.507 (4) | C17B—C18B | 1.374 (4) |
C16A—C17A | 1.372 (4) | C17B—H17B | 0.9300 |
C16A—H16A | 0.9300 | C18B—C19B | 1.382 (4) |
C17A—C18A | 1.390 (4) | C18B—H18B | 0.9300 |
C17A—H17A | 0.9300 | C19B—H19B | 0.9300 |
C18A—C19A | 1.389 (4) | C20B—C21B | 1.401 (3) |
C18A—H18A | 0.9300 | C20B—C25B | 1.407 (3) |
C19A—H19A | 0.9300 | C21B—C22B | 1.398 (3) |
C20A—C25A | 1.394 (4) | C21B—C29B | 1.517 (4) |
C20A—C21A | 1.404 (4) | C22B—C23B | 1.376 (4) |
C21A—C22A | 1.394 (4) | C22B—H22B | 0.9300 |
C21A—C29A | 1.513 (5) | C23B—C24B | 1.389 (4) |
C22A—C23A | 1.391 (5) | C23B—H23B | 0.9300 |
C22A—H22A | 0.9300 | C24B—C25B | 1.386 (4) |
C23A—C24A | 1.368 (5) | C24B—H24B | 0.9300 |
C23A—H23A | 0.9300 | C25B—H25B | 0.9300 |
C24A—C25A | 1.395 (4) | C26B—H26D | 0.9600 |
C24A—H24A | 0.9300 | C26B—H26E | 0.9600 |
C25A—H25A | 0.9300 | C26B—H26F | 0.9600 |
C26A—H26A | 0.9600 | C27B—H27D | 0.9600 |
C26A—H26B | 0.9600 | C27B—H27E | 0.9600 |
C26A—H26C | 0.9600 | C27B—H27F | 0.9600 |
C27A—H27A | 0.9600 | C28B—H28D | 0.9600 |
C27A—H27B | 0.9600 | C28B—H28E | 0.9600 |
C27A—H27C | 0.9600 | C28B—H28F | 0.9600 |
C28A—H28A | 0.9600 | C29B—H29D | 0.9600 |
C28A—H28B | 0.9600 | C29B—H29E | 0.9600 |
C28A—H28C | 0.9600 | C29B—H29F | 0.9600 |
C29A—H29A | 0.9600 | O11—C40 | 1.452 (9) |
C29A—H29B | 0.9600 | O11—H11O | 0.8200 |
C29A—H29C | 0.9600 | C40—H40A | 0.9600 |
Ru1B—C32B | 1.894 (3) | C40—H40B | 0.9600 |
Ru1B—C30B | 1.931 (3) | C40—H40C | 0.9600 |
Ru1B—C31B | 1.936 (3) | ||
C32A—Ru1A—C30A | 88.63 (11) | C30B—Ru1B—P1B | 91.44 (8) |
C32A—Ru1A—C31A | 91.96 (11) | C31B—Ru1B—P1B | 95.74 (8) |
C30A—Ru1A—C31A | 173.81 (11) | C32B—Ru1B—Ru2B | 165.78 (8) |
C32A—Ru1A—P1A | 103.18 (8) | C30B—Ru1B—Ru2B | 95.00 (8) |
C30A—Ru1A—P1A | 91.17 (8) | C31B—Ru1B—Ru2B | 83.35 (7) |
C31A—Ru1A—P1A | 94.69 (8) | P1B—Ru1B—Ru2B | 91.367 (17) |
C32A—Ru1A—Ru2A | 162.77 (8) | C32B—Ru1B—Ru3B | 107.27 (8) |
C30A—Ru1A—Ru2A | 96.43 (8) | C30B—Ru1B—Ru3B | 82.15 (8) |
C31A—Ru1A—Ru2A | 81.29 (7) | C31B—Ru1B—Ru3B | 90.87 (7) |
P1A—Ru1A—Ru2A | 93.205 (17) | P1B—Ru1B—Ru3B | 149.568 (17) |
C32A—Ru1A—Ru3A | 104.63 (8) | Ru2B—Ru1B—Ru3B | 59.886 (7) |
C30A—Ru1A—Ru3A | 84.31 (8) | C35B—Ru2B—C34B | 89.26 (11) |
C31A—Ru1A—Ru3A | 89.57 (7) | C35B—Ru2B—C33B | 91.97 (11) |
P1A—Ru1A—Ru3A | 151.682 (18) | C34B—Ru2B—C33B | 175.99 (11) |
Ru2A—Ru1A—Ru3A | 59.755 (7) | C35B—Ru2B—P2B | 105.74 (8) |
C35A—Ru2A—C33A | 92.38 (11) | C34B—Ru2B—P2B | 89.41 (7) |
C35A—Ru2A—C34A | 89.15 (11) | C33B—Ru2B—P2B | 93.92 (8) |
C33A—Ru2A—C34A | 176.84 (11) | C35B—Ru2B—Ru1B | 160.45 (8) |
C35A—Ru2A—P2A | 106.36 (9) | C34B—Ru2B—Ru1B | 93.99 (7) |
C33A—Ru2A—P2A | 91.90 (8) | C33B—Ru2B—Ru1B | 83.58 (7) |
C34A—Ru2A—P2A | 90.32 (8) | P2B—Ru2B—Ru1B | 93.579 (17) |
C35A—Ru2A—Ru3A | 101.80 (9) | C35B—Ru2B—Ru3B | 101.25 (8) |
C33A—Ru2A—Ru3A | 93.94 (8) | C34B—Ru2B—Ru3B | 82.08 (7) |
C34A—Ru2A—Ru3A | 83.04 (8) | C33B—Ru2B—Ru3B | 93.94 (8) |
P2A—Ru2A—Ru3A | 150.948 (18) | P2B—Ru2B—Ru3B | 151.558 (18) |
C35A—Ru2A—Ru1A | 160.20 (9) | Ru1B—Ru2B—Ru3B | 60.275 (7) |
C33A—Ru2A—Ru1A | 81.39 (7) | C38B—Ru3B—C39B | 104.77 (13) |
C34A—Ru2A—Ru1A | 96.26 (8) | C38B—Ru3B—C36B | 93.83 (13) |
P2A—Ru2A—Ru1A | 92.682 (17) | C39B—Ru3B—C36B | 88.26 (13) |
Ru3A—Ru2A—Ru1A | 60.246 (7) | C38B—Ru3B—C37B | 91.40 (12) |
C38A—Ru3A—C39A | 106.69 (14) | C39B—Ru3B—C37B | 89.77 (12) |
C38A—Ru3A—C36A | 92.55 (13) | C36B—Ru3B—C37B | 174.73 (12) |
C39A—Ru3A—C36A | 89.22 (14) | C38B—Ru3B—Ru2B | 152.18 (9) |
C38A—Ru3A—C37A | 92.02 (12) | C39B—Ru3B—Ru2B | 102.29 (9) |
C39A—Ru3A—C37A | 88.92 (13) | C36B—Ru3B—Ru2B | 80.57 (9) |
C36A—Ru3A—C37A | 175.40 (13) | C37B—Ru3B—Ru2B | 95.08 (8) |
C38A—Ru3A—Ru2A | 151.28 (9) | C38B—Ru3B—Ru1B | 93.62 (8) |
C39A—Ru3A—Ru2A | 101.28 (10) | C39B—Ru3B—Ru1B | 161.40 (9) |
C36A—Ru3A—Ru2A | 81.29 (9) | C36B—Ru3B—Ru1B | 93.28 (9) |
C37A—Ru3A—Ru2A | 94.94 (8) | C37B—Ru3B—Ru1B | 87.04 (8) |
C38A—Ru3A—Ru1A | 92.61 (9) | Ru2B—Ru3B—Ru1B | 59.839 (8) |
C39A—Ru3A—Ru1A | 160.47 (10) | C1B—P1B—C13B | 104.00 (12) |
C36A—Ru3A—Ru1A | 92.96 (9) | C1B—P1B—C7B | 107.70 (11) |
C37A—Ru3A—Ru1A | 87.40 (8) | C13B—P1B—C7B | 96.33 (11) |
Ru2A—Ru3A—Ru1A | 59.999 (8) | C1B—P1B—Ru1B | 112.59 (8) |
C7A—P1A—C1A | 106.67 (11) | C13B—P1B—Ru1B | 114.74 (8) |
C7A—P1A—C13A | 102.74 (11) | C7B—P1B—Ru1B | 119.41 (8) |
C1A—P1A—C13A | 99.85 (12) | C14B—P2B—C20B | 105.50 (11) |
C7A—P1A—Ru1A | 112.52 (8) | C14B—P2B—C13B | 100.68 (12) |
C1A—P1A—Ru1A | 118.21 (8) | C20B—P2B—C13B | 103.39 (11) |
C13A—P1A—Ru1A | 115.05 (8) | C14B—P2B—Ru2B | 119.59 (9) |
C14A—P2A—C13A | 104.04 (12) | C20B—P2B—Ru2B | 111.42 (8) |
C14A—P2A—C20A | 107.04 (12) | C13B—P2B—Ru2B | 114.50 (8) |
C13A—P2A—C20A | 99.22 (12) | C6B—C1B—C2B | 119.4 (2) |
C14A—P2A—Ru2A | 113.14 (8) | C6B—C1B—P1B | 119.59 (19) |
C13A—P2A—Ru2A | 114.00 (8) | C2B—C1B—P1B | 120.94 (19) |
C20A—P2A—Ru2A | 117.72 (10) | C3B—C2B—C1B | 118.2 (2) |
C6A—C1A—C2A | 119.0 (2) | C3B—C2B—C26B | 118.7 (2) |
C6A—C1A—P1A | 117.20 (19) | C1B—C2B—C26B | 123.1 (2) |
C2A—C1A—P1A | 123.71 (19) | C4B—C3B—C2B | 121.9 (3) |
C3A—C2A—C1A | 117.7 (3) | C4B—C3B—H3BA | 119.1 |
C3A—C2A—C26A | 117.7 (2) | C2B—C3B—H3BA | 119.1 |
C1A—C2A—C26A | 124.6 (2) | C3B—C4B—C5B | 119.9 (3) |
C4A—C3A—C2A | 122.4 (3) | C3B—C4B—H4BA | 120.1 |
C4A—C3A—H3AA | 118.8 | C5B—C4B—H4BA | 120.1 |
C2A—C3A—H3AA | 118.8 | C4B—C5B—C6B | 119.3 (3) |
C5A—C4A—C3A | 120.0 (3) | C4B—C5B—H5BA | 120.3 |
C5A—C4A—H4AA | 120.0 | C6B—C5B—H5BA | 120.3 |
C3A—C4A—H4AA | 120.0 | C5B—C6B—C1B | 121.4 (3) |
C4A—C5A—C6A | 118.9 (3) | C5B—C6B—H6BA | 119.3 |
C4A—C5A—H5AA | 120.6 | C1B—C6B—H6BA | 119.3 |
C6A—C5A—H5AA | 120.6 | C12B—C7B—C8B | 119.2 (2) |
C5A—C6A—C1A | 122.1 (2) | C12B—C7B—P1B | 114.88 (18) |
C5A—C6A—H6AA | 119.0 | C8B—C7B—P1B | 125.31 (19) |
C1A—C6A—H6AA | 119.0 | C9B—C8B—C7B | 117.6 (2) |
C12A—C7A—C8A | 119.1 (2) | C9B—C8B—C27B | 117.5 (2) |
C12A—C7A—P1A | 119.11 (19) | C7B—C8B—C27B | 124.9 (2) |
C8A—C7A—P1A | 121.65 (18) | C8B—C9B—C10B | 123.0 (3) |
C9A—C8A—C7A | 118.0 (2) | C8B—C9B—H9BA | 118.5 |
C9A—C8A—C27A | 118.3 (2) | C10B—C9B—H9BA | 118.5 |
C7A—C8A—C27A | 123.7 (2) | C11B—C10B—C9B | 119.1 (3) |
C10A—C9A—C8A | 122.8 (3) | C11B—C10B—H10B | 120.5 |
C10A—C9A—H9AA | 118.6 | C9B—C10B—H10B | 120.5 |
C8A—C9A—H9AA | 118.6 | C10B—C11B—C12B | 119.2 (3) |
C9A—C10A—C11A | 119.4 (2) | C10B—C11B—H11B | 120.4 |
C9A—C10A—H10A | 120.3 | C12B—C11B—H11B | 120.4 |
C11A—C10A—H10A | 120.3 | C11B—C12B—C7B | 121.9 (2) |
C12A—C11A—C10A | 119.1 (3) | C11B—C12B—H12B | 119.0 |
C12A—C11A—H11A | 120.5 | C7B—C12B—H12B | 119.0 |
C10A—C11A—H11A | 120.5 | P1B—C13B—P2B | 117.59 (14) |
C11A—C12A—C7A | 121.6 (3) | P1B—C13B—H13C | 107.9 |
C11A—C12A—H12A | 119.2 | P2B—C13B—H13C | 107.9 |
C7A—C12A—H12A | 119.2 | P1B—C13B—H13D | 107.9 |
P2A—C13A—P1A | 118.00 (14) | P2B—C13B—H13D | 107.9 |
P2A—C13A—H13A | 107.8 | H13C—C13B—H13D | 107.2 |
P1A—C13A—H13A | 107.8 | C19B—C14B—C15B | 119.1 (2) |
P2A—C13A—H13B | 107.8 | C19B—C14B—P2B | 117.6 (2) |
P1A—C13A—H13B | 107.8 | C15B—C14B—P2B | 123.3 (2) |
H13A—C13A—H13B | 107.1 | C16B—C15B—C14B | 117.6 (3) |
C19A—C14A—C15A | 119.4 (2) | C16B—C15B—C28B | 118.4 (3) |
C19A—C14A—P2A | 119.82 (19) | C14B—C15B—C28B | 124.1 (2) |
C15A—C14A—P2A | 120.64 (19) | C17B—C16B—C15B | 122.6 (3) |
C16A—C15A—C14A | 118.1 (2) | C17B—C16B—H16B | 118.7 |
C16A—C15A—C28A | 118.8 (2) | C15B—C16B—H16B | 118.7 |
C14A—C15A—C28A | 123.0 (2) | C16B—C17B—C18B | 119.9 (3) |
C17A—C16A—C15A | 122.2 (3) | C16B—C17B—H17B | 120.1 |
C17A—C16A—H16A | 118.9 | C18B—C17B—H17B | 120.1 |
C15A—C16A—H16A | 118.9 | C17B—C18B—C19B | 119.4 (3) |
C16A—C17A—C18A | 119.8 (3) | C17B—C18B—H18B | 120.3 |
C16A—C17A—H17A | 120.1 | C19B—C18B—H18B | 120.3 |
C18A—C17A—H17A | 120.1 | C18B—C19B—C14B | 121.4 (3) |
C19A—C18A—C17A | 119.4 (3) | C18B—C19B—H19B | 119.3 |
C19A—C18A—H18A | 120.3 | C14B—C19B—H19B | 119.3 |
C17A—C18A—H18A | 120.3 | C21B—C20B—C25B | 118.8 (2) |
C18A—C19A—C14A | 121.0 (3) | C21B—C20B—P2B | 120.95 (18) |
C18A—C19A—H19A | 119.5 | C25B—C20B—P2B | 120.01 (19) |
C14A—C19A—H19A | 119.5 | C22B—C21B—C20B | 118.6 (2) |
C25A—C20A—C21A | 118.7 (3) | C22B—C21B—C29B | 117.7 (2) |
C25A—C20A—P2A | 115.9 (2) | C20B—C21B—C29B | 123.7 (2) |
C21A—C20A—P2A | 125.3 (2) | C23B—C22B—C21B | 122.3 (3) |
C22A—C21A—C20A | 118.3 (3) | C23B—C22B—H22B | 118.8 |
C22A—C21A—C29A | 118.0 (3) | C21B—C22B—H22B | 118.8 |
C20A—C21A—C29A | 123.7 (3) | C22B—C23B—C24B | 119.2 (3) |
C23A—C22A—C21A | 122.1 (3) | C22B—C23B—H23B | 120.4 |
C23A—C22A—H22A | 118.9 | C24B—C23B—H23B | 120.4 |
C21A—C22A—H22A | 118.9 | C25B—C24B—C23B | 119.7 (3) |
C24A—C23A—C22A | 119.7 (3) | C25B—C24B—H24B | 120.1 |
C24A—C23A—H23A | 120.2 | C23B—C24B—H24B | 120.1 |
C22A—C23A—H23A | 120.2 | C24B—C25B—C20B | 121.3 (3) |
C23A—C24A—C25A | 119.1 (3) | C24B—C25B—H25B | 119.4 |
C23A—C24A—H24A | 120.5 | C20B—C25B—H25B | 119.4 |
C25A—C24A—H24A | 120.5 | C2B—C26B—H26D | 109.5 |
C20A—C25A—C24A | 122.1 (3) | C2B—C26B—H26E | 109.5 |
C20A—C25A—H25A | 118.9 | H26D—C26B—H26E | 109.5 |
C24A—C25A—H25A | 118.9 | C2B—C26B—H26F | 109.5 |
C2A—C26A—H26A | 109.5 | H26D—C26B—H26F | 109.5 |
C2A—C26A—H26B | 109.5 | H26E—C26B—H26F | 109.5 |
H26A—C26A—H26B | 109.5 | C8B—C27B—H27D | 109.5 |
C2A—C26A—H26C | 109.5 | C8B—C27B—H27E | 109.5 |
H26A—C26A—H26C | 109.5 | H27D—C27B—H27E | 109.5 |
H26B—C26A—H26C | 109.5 | C8B—C27B—H27F | 109.5 |
C8A—C27A—H27A | 109.5 | H27D—C27B—H27F | 109.5 |
C8A—C27A—H27B | 109.5 | H27E—C27B—H27F | 109.5 |
H27A—C27A—H27B | 109.5 | C15B—C28B—H28D | 109.5 |
C8A—C27A—H27C | 109.5 | C15B—C28B—H28E | 109.5 |
H27A—C27A—H27C | 109.5 | H28D—C28B—H28E | 109.5 |
H27B—C27A—H27C | 109.5 | C15B—C28B—H28F | 109.5 |
C15A—C28A—H28A | 109.5 | H28D—C28B—H28F | 109.5 |
C15A—C28A—H28B | 109.5 | H28E—C28B—H28F | 109.5 |
H28A—C28A—H28B | 109.5 | C21B—C29B—H29D | 109.5 |
C15A—C28A—H28C | 109.5 | C21B—C29B—H29E | 109.5 |
H28A—C28A—H28C | 109.5 | H29D—C29B—H29E | 109.5 |
H28B—C28A—H28C | 109.5 | C21B—C29B—H29F | 109.5 |
C21A—C29A—H29A | 109.5 | H29D—C29B—H29F | 109.5 |
C21A—C29A—H29B | 109.5 | H29E—C29B—H29F | 109.5 |
H29A—C29A—H29B | 109.5 | O1B—C30B—Ru1B | 172.9 (2) |
C21A—C29A—H29C | 109.5 | O2B—C31B—Ru1B | 173.6 (2) |
H29A—C29A—H29C | 109.5 | O3B—C32B—Ru1B | 178.7 (2) |
H29B—C29A—H29C | 109.5 | O4B—C33B—Ru2B | 173.8 (2) |
O1A—C30A—Ru1A | 173.6 (2) | O5B—C34B—Ru2B | 173.5 (2) |
O2A—C31A—Ru1A | 173.0 (2) | O6B—C35B—Ru2B | 178.1 (3) |
O3A—C32A—Ru1A | 179.4 (3) | O7B—C36B—Ru3B | 171.9 (3) |
O4A—C33A—Ru2A | 173.2 (2) | O8B—C37B—Ru3B | 172.4 (2) |
O5A—C34A—Ru2A | 172.5 (2) | O9B—C38B—Ru3B | 178.4 (3) |
O6A—C35A—Ru2A | 178.7 (3) | O10B—C39B—Ru3B | 178.6 (3) |
O7A—C36A—Ru3A | 172.2 (3) | C40—O11—H11O | 109.5 |
O8A—C37A—Ru3A | 172.4 (3) | O11—C40—H40A | 109.5 |
O9A—C38A—Ru3A | 178.2 (3) | O11—C40—H40B | 109.5 |
O10A—C39A—Ru3A | 179.1 (3) | H40A—C40—H40B | 109.5 |
C32B—Ru1B—C30B | 88.74 (11) | O11—C40—H40C | 109.5 |
C32B—Ru1B—C31B | 91.19 (11) | H40A—C40—H40C | 109.5 |
C30B—Ru1B—C31B | 172.66 (11) | H40B—C40—H40C | 109.5 |
C32B—Ru1B—P1B | 102.27 (8) | ||
C32A—Ru1A—Ru2A—C35A | 53.6 (4) | C32B—Ru1B—Ru2B—C35B | −47.5 (4) |
C30A—Ru1A—Ru2A—C35A | −52.7 (3) | C30B—Ru1B—Ru2B—C35B | 57.3 (3) |
C31A—Ru1A—Ru2A—C35A | 121.5 (3) | C31B—Ru1B—Ru2B—C35B | −115.5 (2) |
P1A—Ru1A—Ru2A—C35A | −144.3 (2) | P1B—Ru1B—Ru2B—C35B | 148.9 (2) |
Ru3A—Ru1A—Ru2A—C35A | 26.8 (2) | Ru3B—Ru1B—Ru2B—C35B | −20.6 (2) |
C32A—Ru1A—Ru2A—C33A | 126.4 (3) | C32B—Ru1B—Ru2B—C34B | 51.6 (3) |
C30A—Ru1A—Ru2A—C33A | 20.02 (11) | C30B—Ru1B—Ru2B—C34B | 156.44 (11) |
C31A—Ru1A—Ru2A—C33A | −165.78 (11) | C31B—Ru1B—Ru2B—C34B | −16.36 (10) |
P1A—Ru1A—Ru2A—C33A | −71.52 (8) | P1B—Ru1B—Ru2B—C34B | −111.99 (8) |
Ru3A—Ru1A—Ru2A—C33A | 99.59 (8) | Ru3B—Ru1B—Ru2B—C34B | 78.53 (7) |
C32A—Ru1A—Ru2A—C34A | −51.5 (3) | C32B—Ru1B—Ru2B—C33B | −125.2 (3) |
C30A—Ru1A—Ru2A—C34A | −157.84 (11) | C30B—Ru1B—Ru2B—C33B | −20.35 (11) |
C31A—Ru1A—Ru2A—C34A | 16.35 (11) | C31B—Ru1B—Ru2B—C33B | 166.84 (11) |
P1A—Ru1A—Ru2A—C34A | 110.61 (8) | P1B—Ru1B—Ru2B—C33B | 71.22 (8) |
Ru3A—Ru1A—Ru2A—C34A | −78.28 (8) | Ru3B—Ru1B—Ru2B—C33B | −98.27 (8) |
C32A—Ru1A—Ru2A—P2A | −142.1 (3) | C32B—Ru1B—Ru2B—P2B | 141.3 (3) |
C30A—Ru1A—Ru2A—P2A | 111.54 (8) | C30B—Ru1B—Ru2B—P2B | −113.90 (8) |
C31A—Ru1A—Ru2A—P2A | −74.27 (8) | C31B—Ru1B—Ru2B—P2B | 73.29 (8) |
P1A—Ru1A—Ru2A—P2A | 20.00 (2) | P1B—Ru1B—Ru2B—P2B | −22.33 (2) |
Ru3A—Ru1A—Ru2A—P2A | −168.890 (18) | Ru3B—Ru1B—Ru2B—P2B | 168.180 (18) |
C32A—Ru1A—Ru2A—Ru3A | 26.8 (3) | C32B—Ru1B—Ru2B—Ru3B | −26.9 (3) |
C30A—Ru1A—Ru2A—Ru3A | −79.57 (8) | C30B—Ru1B—Ru2B—Ru3B | 77.92 (8) |
C31A—Ru1A—Ru2A—Ru3A | 94.62 (8) | C31B—Ru1B—Ru2B—Ru3B | −94.89 (7) |
P1A—Ru1A—Ru2A—Ru3A | −171.113 (17) | P1B—Ru1B—Ru2B—Ru3B | 169.488 (18) |
C35A—Ru2A—Ru3A—C38A | −151.75 (19) | C35B—Ru2B—Ru3B—C38B | 153.9 (2) |
C33A—Ru2A—Ru3A—C38A | −58.48 (19) | C34B—Ru2B—Ru3B—C38B | −118.4 (2) |
C34A—Ru2A—Ru3A—C38A | 120.59 (19) | C33B—Ru2B—Ru3B—C38B | 61.1 (2) |
P2A—Ru2A—Ru3A—C38A | 42.61 (18) | P2B—Ru2B—Ru3B—C38B | −44.60 (19) |
Ru1A—Ru2A—Ru3A—C38A | 19.26 (17) | Ru1B—Ru2B—Ru3B—C38B | −19.18 (18) |
C35A—Ru2A—Ru3A—C39A | 14.99 (13) | C35B—Ru2B—Ru3B—C39B | −12.43 (12) |
C33A—Ru2A—Ru3A—C39A | 108.25 (13) | C34B—Ru2B—Ru3B—C39B | 75.23 (12) |
C34A—Ru2A—Ru3A—C39A | −72.68 (13) | C33B—Ru2B—Ru3B—C39B | −105.23 (12) |
P2A—Ru2A—Ru3A—C39A | −150.65 (11) | P2B—Ru2B—Ru3B—C39B | 149.04 (10) |
Ru1A—Ru2A—Ru3A—C39A | −174.00 (10) | Ru1B—Ru2B—Ru3B—C39B | 174.46 (10) |
C35A—Ru2A—Ru3A—C36A | −72.46 (12) | C35B—Ru2B—Ru3B—C36B | 73.70 (12) |
C33A—Ru2A—Ru3A—C36A | 20.81 (12) | C34B—Ru2B—Ru3B—C36B | 161.35 (12) |
C34A—Ru2A—Ru3A—C36A | −160.12 (12) | C33B—Ru2B—Ru3B—C36B | −19.11 (12) |
P2A—Ru2A—Ru3A—C36A | 121.90 (10) | P2B—Ru2B—Ru3B—C36B | −124.84 (10) |
Ru1A—Ru2A—Ru3A—C36A | 98.55 (9) | Ru1B—Ru2B—Ru3B—C36B | −99.42 (10) |
C35A—Ru2A—Ru3A—C37A | 104.87 (12) | C35B—Ru2B—Ru3B—C37B | −103.30 (11) |
C33A—Ru2A—Ru3A—C37A | −161.86 (11) | C34B—Ru2B—Ru3B—C37B | −15.64 (11) |
C34A—Ru2A—Ru3A—C37A | 17.21 (11) | C33B—Ru2B—Ru3B—C37B | 163.90 (11) |
P2A—Ru2A—Ru3A—C37A | −60.77 (9) | P2B—Ru2B—Ru3B—C37B | 58.17 (9) |
Ru1A—Ru2A—Ru3A—C37A | −84.12 (8) | Ru1B—Ru2B—Ru3B—C37B | 83.59 (8) |
C35A—Ru2A—Ru3A—Ru1A | −171.01 (8) | C35B—Ru2B—Ru3B—Ru1B | 173.11 (8) |
C33A—Ru2A—Ru3A—Ru1A | −77.74 (7) | C34B—Ru2B—Ru3B—Ru1B | −99.23 (7) |
C34A—Ru2A—Ru3A—Ru1A | 101.33 (7) | C33B—Ru2B—Ru3B—Ru1B | 80.31 (7) |
P2A—Ru2A—Ru3A—Ru1A | 23.35 (4) | P2B—Ru2B—Ru3B—Ru1B | −25.42 (4) |
C32A—Ru1A—Ru3A—C38A | 17.06 (12) | C32B—Ru1B—Ru3B—C38B | −15.52 (12) |
C30A—Ru1A—Ru3A—C38A | −70.02 (11) | C30B—Ru1B—Ru3B—C38B | 70.69 (12) |
C31A—Ru1A—Ru3A—C38A | 108.97 (11) | C31B—Ru1B—Ru3B—C38B | −107.04 (11) |
P1A—Ru1A—Ru3A—C38A | −151.89 (9) | P1B—Ru1B—Ru3B—C38B | 150.06 (9) |
Ru2A—Ru1A—Ru3A—C38A | −170.87 (8) | Ru2B—Ru1B—Ru3B—C38B | 171.16 (9) |
C32A—Ru1A—Ru3A—C39A | −154.2 (3) | C32B—Ru1B—Ru3B—C39B | 156.1 (3) |
C30A—Ru1A—Ru3A—C39A | 118.7 (3) | C30B—Ru1B—Ru3B—C39B | −117.7 (3) |
C31A—Ru1A—Ru3A—C39A | −62.3 (3) | C31B—Ru1B—Ru3B—C39B | 64.6 (3) |
P1A—Ru1A—Ru3A—C39A | 36.8 (3) | P1B—Ru1B—Ru3B—C39B | −38.3 (3) |
Ru2A—Ru1A—Ru3A—C39A | 17.8 (3) | Ru2B—Ru1B—Ru3B—C39B | −17.2 (3) |
C32A—Ru1A—Ru3A—C36A | 109.75 (12) | C32B—Ru1B—Ru3B—C36B | −109.58 (12) |
C30A—Ru1A—Ru3A—C36A | 22.67 (12) | C30B—Ru1B—Ru3B—C36B | −23.36 (12) |
C31A—Ru1A—Ru3A—C36A | −158.34 (12) | C31B—Ru1B—Ru3B—C36B | 158.91 (12) |
P1A—Ru1A—Ru3A—C36A | −59.20 (10) | P1B—Ru1B—Ru3B—C36B | 56.00 (10) |
Ru2A—Ru1A—Ru3A—C36A | −78.18 (10) | Ru2B—Ru1B—Ru3B—C36B | 77.11 (9) |
C32A—Ru1A—Ru3A—C37A | −74.84 (11) | C32B—Ru1B—Ru3B—C37B | 75.69 (11) |
C30A—Ru1A—Ru3A—C37A | −161.92 (11) | C30B—Ru1B—Ru3B—C37B | 161.91 (11) |
C31A—Ru1A—Ru3A—C37A | 17.07 (11) | C31B—Ru1B—Ru3B—C37B | −15.82 (11) |
P1A—Ru1A—Ru3A—C37A | 116.20 (9) | P1B—Ru1B—Ru3B—C37B | −118.73 (9) |
Ru2A—Ru1A—Ru3A—C37A | 97.23 (8) | Ru2B—Ru1B—Ru3B—C37B | −97.62 (8) |
C32A—Ru1A—Ru3A—Ru2A | −172.07 (8) | C32B—Ru1B—Ru3B—Ru2B | 173.32 (8) |
C30A—Ru1A—Ru3A—Ru2A | 100.85 (8) | C30B—Ru1B—Ru3B—Ru2B | −100.47 (8) |
C31A—Ru1A—Ru3A—Ru2A | −80.16 (8) | C31B—Ru1B—Ru3B—Ru2B | 81.80 (8) |
P1A—Ru1A—Ru3A—Ru2A | 18.98 (4) | P1B—Ru1B—Ru3B—Ru2B | −21.10 (3) |
C32A—Ru1A—P1A—C7A | −81.13 (12) | C32B—Ru1B—P1B—C1B | 93.21 (12) |
C30A—Ru1A—P1A—C7A | 7.74 (11) | C30B—Ru1B—P1B—C1B | 4.18 (12) |
C31A—Ru1A—P1A—C7A | −174.25 (11) | C31B—Ru1B—P1B—C1B | −174.31 (11) |
Ru2A—Ru1A—P1A—C7A | 104.24 (9) | Ru2B—Ru1B—P1B—C1B | −90.86 (9) |
Ru3A—Ru1A—P1A—C7A | 87.90 (9) | Ru3B—Ru1B—P1B—C1B | −72.70 (10) |
C32A—Ru1A—P1A—C1A | 43.95 (12) | C32B—Ru1B—P1B—C13B | −148.09 (12) |
C30A—Ru1A—P1A—C1A | 132.82 (12) | C30B—Ru1B—P1B—C13B | 122.88 (12) |
C31A—Ru1A—P1A—C1A | −49.17 (12) | C31B—Ru1B—P1B—C13B | −55.61 (12) |
Ru2A—Ru1A—P1A—C1A | −130.68 (9) | Ru2B—Ru1B—P1B—C13B | 27.84 (10) |
Ru3A—Ru1A—P1A—C1A | −147.02 (9) | Ru3B—Ru1B—P1B—C13B | 46.00 (11) |
C32A—Ru1A—P1A—C13A | 161.67 (12) | C32B—Ru1B—P1B—C7B | −34.56 (12) |
C30A—Ru1A—P1A—C13A | −109.47 (12) | C30B—Ru1B—P1B—C7B | −123.59 (12) |
C31A—Ru1A—P1A—C13A | 68.54 (12) | C31B—Ru1B—P1B—C7B | 57.91 (12) |
Ru2A—Ru1A—P1A—C13A | −12.97 (9) | Ru2B—Ru1B—P1B—C7B | 141.37 (9) |
Ru3A—Ru1A—P1A—C13A | −29.31 (11) | Ru3B—Ru1B—P1B—C7B | 159.52 (9) |
C35A—Ru2A—P2A—C14A | −93.15 (12) | C35B—Ru2B—P2B—C14B | −41.26 (12) |
C33A—Ru2A—P2A—C14A | 173.81 (11) | C34B—Ru2B—P2B—C14B | −130.33 (12) |
C34A—Ru2A—P2A—C14A | −3.94 (12) | C33B—Ru2B—P2B—C14B | 51.90 (12) |
Ru3A—Ru2A—P2A—C14A | 72.19 (10) | Ru1B—Ru2B—P2B—C14B | 135.70 (9) |
Ru1A—Ru2A—P2A—C14A | 92.34 (9) | Ru3B—Ru2B—P2B—C14B | 157.64 (9) |
C35A—Ru2A—P2A—C13A | 148.23 (12) | C35B—Ru2B—P2B—C20B | 82.31 (12) |
C33A—Ru2A—P2A—C13A | 55.18 (12) | C34B—Ru2B—P2B—C20B | −6.76 (11) |
C34A—Ru2A—P2A—C13A | −122.56 (12) | C33B—Ru2B—P2B—C20B | 175.47 (11) |
Ru3A—Ru2A—P2A—C13A | −46.43 (10) | Ru1B—Ru2B—P2B—C20B | −100.73 (9) |
Ru1A—Ru2A—P2A—C13A | −26.28 (9) | Ru3B—Ru2B—P2B—C20B | −78.79 (9) |
C35A—Ru2A—P2A—C20A | 32.63 (13) | C35B—Ru2B—P2B—C13B | −160.80 (12) |
C33A—Ru2A—P2A—C20A | −60.41 (12) | C34B—Ru2B—P2B—C13B | 110.13 (12) |
C34A—Ru2A—P2A—C20A | 121.84 (12) | C33B—Ru2B—P2B—C13B | −67.64 (12) |
Ru3A—Ru2A—P2A—C20A | −162.03 (9) | Ru1B—Ru2B—P2B—C13B | 16.16 (10) |
Ru1A—Ru2A—P2A—C20A | −141.87 (10) | Ru3B—Ru2B—P2B—C13B | 38.09 (11) |
C7A—P1A—C1A—C6A | 135.0 (2) | C13B—P1B—C1B—C6B | −24.2 (2) |
C13A—P1A—C1A—C6A | −118.4 (2) | C7B—P1B—C1B—C6B | −125.7 (2) |
Ru1A—P1A—C1A—C6A | 7.1 (2) | Ru1B—P1B—C1B—C6B | 100.6 (2) |
C7A—P1A—C1A—C2A | −49.2 (2) | C13B—P1B—C1B—C2B | 159.3 (2) |
C13A—P1A—C1A—C2A | 57.4 (2) | C7B—P1B—C1B—C2B | 57.9 (2) |
Ru1A—P1A—C1A—C2A | −177.12 (19) | Ru1B—P1B—C1B—C2B | −75.9 (2) |
C6A—C1A—C2A—C3A | 1.9 (4) | C6B—C1B—C2B—C3B | 3.0 (4) |
P1A—C1A—C2A—C3A | −173.7 (2) | P1B—C1B—C2B—C3B | 179.48 (19) |
C6A—C1A—C2A—C26A | −175.1 (3) | C6B—C1B—C2B—C26B | −178.9 (3) |
P1A—C1A—C2A—C26A | 9.2 (4) | P1B—C1B—C2B—C26B | −2.4 (4) |
C1A—C2A—C3A—C4A | 0.2 (4) | C1B—C2B—C3B—C4B | −2.2 (4) |
C26A—C2A—C3A—C4A | 177.4 (3) | C26B—C2B—C3B—C4B | 179.6 (3) |
C2A—C3A—C4A—C5A | −2.0 (5) | C2B—C3B—C4B—C5B | 0.0 (4) |
C3A—C4A—C5A—C6A | 1.7 (4) | C3B—C4B—C5B—C6B | 1.4 (4) |
C4A—C5A—C6A—C1A | 0.5 (4) | C4B—C5B—C6B—C1B | −0.5 (4) |
C2A—C1A—C6A—C5A | −2.3 (4) | C2B—C1B—C6B—C5B | −1.7 (4) |
P1A—C1A—C6A—C5A | 173.6 (2) | P1B—C1B—C6B—C5B | −178.2 (2) |
C1A—P1A—C7A—C12A | 135.6 (2) | C1B—P1B—C7B—C12B | −152.72 (19) |
C13A—P1A—C7A—C12A | 31.1 (2) | C13B—P1B—C7B—C12B | 100.4 (2) |
Ru1A—P1A—C7A—C12A | −93.2 (2) | Ru1B—P1B—C7B—C12B | −22.7 (2) |
C1A—P1A—C7A—C8A | −48.8 (2) | C1B—P1B—C7B—C8B | 36.6 (2) |
C13A—P1A—C7A—C8A | −153.3 (2) | C13B—P1B—C7B—C8B | −70.3 (2) |
Ru1A—P1A—C7A—C8A | 82.4 (2) | Ru1B—P1B—C7B—C8B | 166.63 (18) |
C12A—C7A—C8A—C9A | −2.9 (4) | C12B—C7B—C8B—C9B | −0.7 (4) |
P1A—C7A—C8A—C9A | −178.5 (2) | P1B—C7B—C8B—C9B | 169.6 (2) |
C12A—C7A—C8A—C27A | 177.3 (3) | C12B—C7B—C8B—C27B | −179.9 (2) |
P1A—C7A—C8A—C27A | 1.7 (4) | P1B—C7B—C8B—C27B | −9.6 (4) |
C7A—C8A—C9A—C10A | 1.1 (4) | C7B—C8B—C9B—C10B | −0.9 (4) |
C27A—C8A—C9A—C10A | −179.0 (3) | C27B—C8B—C9B—C10B | 178.3 (3) |
C8A—C9A—C10A—C11A | 1.4 (4) | C8B—C9B—C10B—C11B | 1.2 (4) |
C9A—C10A—C11A—C12A | −2.2 (4) | C9B—C10B—C11B—C12B | 0.2 (4) |
C10A—C11A—C12A—C7A | 0.4 (4) | C10B—C11B—C12B—C7B | −1.9 (4) |
C8A—C7A—C12A—C11A | 2.2 (4) | C8B—C7B—C12B—C11B | 2.2 (4) |
P1A—C7A—C12A—C11A | 177.9 (2) | P1B—C7B—C12B—C11B | −169.1 (2) |
C14A—P2A—C13A—P1A | −100.89 (16) | C1B—P1B—C13B—P2B | 100.90 (16) |
C20A—P2A—C13A—P1A | 148.82 (15) | C7B—P1B—C13B—P2B | −149.05 (15) |
Ru2A—P2A—C13A—P1A | 22.80 (18) | Ru1B—P1B—C13B—P2B | −22.53 (18) |
C7A—P1A—C13A—P2A | −125.87 (15) | C14B—P2B—C13B—P1B | −129.22 (15) |
C1A—P1A—C13A—P2A | 124.39 (15) | C20B—P2B—C13B—P1B | 121.84 (15) |
Ru1A—P1A—C13A—P2A | −3.25 (18) | Ru2B—P2B—C13B—P1B | 0.44 (18) |
C13A—P2A—C14A—C19A | 23.7 (2) | C20B—P2B—C14B—C19B | −132.4 (2) |
C20A—P2A—C14A—C19A | 128.2 (2) | C13B—P2B—C14B—C19B | 120.3 (2) |
Ru2A—P2A—C14A—C19A | −100.5 (2) | Ru2B—P2B—C14B—C19B | −6.0 (2) |
C13A—P2A—C14A—C15A | −160.4 (2) | C20B—P2B—C14B—C15B | 48.4 (2) |
C20A—P2A—C14A—C15A | −56.0 (2) | C13B—P2B—C14B—C15B | −58.9 (2) |
Ru2A—P2A—C14A—C15A | 75.3 (2) | Ru2B—P2B—C14B—C15B | 174.80 (18) |
C19A—C14A—C15A—C16A | −3.0 (4) | C19B—C14B—C15B—C16B | 0.5 (4) |
P2A—C14A—C15A—C16A | −178.8 (2) | P2B—C14B—C15B—C16B | 179.7 (2) |
C19A—C14A—C15A—C28A | 178.8 (3) | C19B—C14B—C15B—C28B | −179.6 (3) |
P2A—C14A—C15A—C28A | 2.9 (4) | P2B—C14B—C15B—C28B | −0.4 (4) |
C14A—C15A—C16A—C17A | 1.6 (4) | C14B—C15B—C16B—C17B | −1.0 (5) |
C28A—C15A—C16A—C17A | 180.0 (3) | C28B—C15B—C16B—C17B | 179.1 (3) |
C15A—C16A—C17A—C18A | 0.8 (5) | C15B—C16B—C17B—C18B | 0.1 (5) |
C16A—C17A—C18A—C19A | −1.9 (4) | C16B—C17B—C18B—C19B | 1.3 (5) |
C17A—C18A—C19A—C14A | 0.5 (4) | C17B—C18B—C19B—C14B | −1.8 (5) |
C15A—C14A—C19A—C18A | 1.9 (4) | C15B—C14B—C19B—C18B | 0.9 (4) |
P2A—C14A—C19A—C18A | 177.8 (2) | P2B—C14B—C19B—C18B | −178.4 (2) |
C14A—P2A—C20A—C25A | 143.5 (2) | C14B—P2B—C20B—C21B | 51.6 (2) |
C13A—P2A—C20A—C25A | −108.7 (2) | C13B—P2B—C20B—C21B | 156.9 (2) |
Ru2A—P2A—C20A—C25A | 14.7 (2) | Ru2B—P2B—C20B—C21B | −79.6 (2) |
C14A—P2A—C20A—C21A | −41.6 (3) | C14B—P2B—C20B—C25B | −134.1 (2) |
C13A—P2A—C20A—C21A | 66.3 (3) | C13B—P2B—C20B—C25B | −28.8 (2) |
Ru2A—P2A—C20A—C21A | −170.3 (2) | Ru2B—P2B—C20B—C25B | 94.7 (2) |
C25A—C20A—C21A—C22A | −2.5 (5) | C25B—C20B—C21B—C22B | 2.1 (4) |
P2A—C20A—C21A—C22A | −177.4 (3) | P2B—C20B—C21B—C22B | 176.54 (19) |
C25A—C20A—C21A—C29A | 178.0 (3) | C25B—C20B—C21B—C29B | −177.0 (2) |
P2A—C20A—C21A—C29A | 3.2 (5) | P2B—C20B—C21B—C29B | −2.7 (4) |
C20A—C21A—C22A—C23A | 2.9 (6) | C20B—C21B—C22B—C23B | −1.1 (4) |
C29A—C21A—C22A—C23A | −177.7 (4) | C29B—C21B—C22B—C23B | 178.1 (3) |
C21A—C22A—C23A—C24A | −0.9 (6) | C21B—C22B—C23B—C24B | −0.4 (4) |
C22A—C23A—C24A—C25A | −1.4 (5) | C22B—C23B—C24B—C25B | 0.8 (4) |
C21A—C20A—C25A—C24A | 0.3 (4) | C23B—C24B—C25B—C20B | 0.3 (4) |
P2A—C20A—C25A—C24A | 175.6 (2) | C21B—C20B—C25B—C24B | −1.8 (4) |
C23A—C24A—C25A—C20A | 1.7 (4) | P2B—C20B—C25B—C24B | −176.2 (2) |
Cg1 is centroid of the C14A–C19A benzene ring. |
D—H···A | D—H | H···A | D···A | D—H···A |
C11B—H11B···O1Bi | 0.93 | 2.54 | 3.251 (3) | 134 |
C24A—H24A···O5Aii | 0.93 | 2.49 | 3.240 (4) | 138 |
C29A—H29B···Cg1 | 0.96 | 2.96 | 3.702 (4) | 135 |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+3/2, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | 8[Ru3(C29H30P2)(CO)10]·CH4O |
Mr | 8222.28 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 100 |
a, b, c (Å) | 22.7156 (13), 19.9023 (11), 18.4979 (10) |
β (°) | 106.561 (1) |
V (Å3) | 8015.8 (8) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.25 |
Crystal size (mm) | 0.23 × 0.10 × 0.06 |
Data collection | |
Diffractometer | Bruker APEXII DUO CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2009) |
Tmin, Tmax | 0.758, 0.932 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 107136, 28473, 20091 |
Rint | 0.056 |
(sin θ/λ)max (Å−1) | 0.755 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.035, 0.082, 1.03 |
No. of reflections | 28473 |
No. of parameters | 990 |
No. of restraints | 1 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.14, −0.72 |
Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).
Ru1A—P1A | 2.3451 (7) | Ru1B—P1B | 2.3450 (7) |
Ru2A—P2A | 2.3422 (7) | Ru2B—P2B | 2.3459 (7) |
Cg1 is centroid of the C14A–C19A benzene ring. |
D—H···A | D—H | H···A | D···A | D—H···A |
C11B—H11B···O1Bi | 0.93 | 2.54 | 3.251 (3) | 134 |
C24A—H24A···O5Aii | 0.93 | 2.49 | 3.240 (4) | 138 |
C29A—H29B···Cg1 | 0.96 | 2.96 | 3.702 (4) | 135 |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+3/2, z+1/2. |
Footnotes
‡Thomson Reuters ResearcherID: B-6034-2009. On secondment to: Multimedia University, Melaka Campus, Jalan Ayer Keroh Lama, 74750 Melaka, Malaysia.
§Thomson Reuters ResearcherID: E-2833-2010. Current address: Department of Chemistry, Gokhale Centenary College, Ankola 581 314, NK, Karnataka, India.
¶Thomson Reuters ResearcherID: A-5523-2009.
‡‡Thomson Reuters ResearcherID: A-3561-2009. Additional correspondence author, e-mail: hkfun@usm.my.
Acknowledgements
The authors would like to thank the Malaysian Government and Universiti Sains Malaysia (USM) for the Research Grant 1001/PJJAUH/811115. IAK is grateful to USM for a Visiting Researcher position. HKF and CSY thank USM for the Research University Grant No. 1001/PFIZIK/811160.
References
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This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
A large number of substituted derivatives, Ru3(CO)12-nLn (L = group 15 ligand) have been reported (Bruce et al., 1985, 1988a,b; Bruce et al., 1985). As part of our study on the substitution of transition metal-carbonyl clusters with mixed-ligand complexes, we have published several structures of triangulo-triruthenium-carbonyl clusters containing mixed P/As and P/Sb ligands (Shawkataly et al., 1998, 2004, 2010). Herein we report the synthesis and structure of the title compound.
The asymmetry unit of title compound consists of two molecule of triangulo-triruthenium complex (A & B) and one-quater molecule of methanol solvent (Fig. 1). The bis(di-o-tolylphosphanyl)methane ligand bridges the Ru1–Ru2 bond. The phosphine ligand is equatorial with respect to the Ru triangle. The Ru1 and Ru2 atoms each carries one equatorial and two axial terminal carbonyl ligands whereas the Ru3 atom carries two equatorial and two axial terminal carbonyl ligands. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 76.26 (13) and 74.76 (15)° in molecule A for the two diphenylphosphanyl groups respectively whereas these angles are 77.21 (13) and 75.68 (14)° in molecule B.
In the crystal, the molecules are linked into one-dimensional chains along c axis via intermolecular C11B—H11B···O1B and C24A—H24A···O5A hydrogen bonds (Fig. 2, Table 1). Weak intermolecular C—H···π interactions (Table 1) consolidate the packing.