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Acta Cryst. (2010). E66, m583-m584    [ doi:10.1107/S1600536810013838 ]

Decacarbonyl-1[kappa]3C,2[kappa]3C,3[kappa]4C-bis[tris(3-chlorophenyl)phosphine]-1[kappa]P,2[kappa]P-triangulo-triruthenium(0) monohydrate

O. bin Shawkataly, M. A. A. Pankhi, C. S. Yeap and H.-K. Fun

Abstract top

The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C18H12Cl3P)2(CO)10]·H2O, consists of one triangulo-triruthenium complex and one disordered water solvent molecule. Two of the 3-chlorophenyl rings are disordered over two positions with refined site occupancies of 0.671 (3)/0.329 (3) and 0.628 (3)/0.372 (3). The water molecule is disordered over two positions with refined site occupancies of 0.523 (7) and 0.477 (7). Two equatorial carbonyl groups have been substituted by the two monodentate phosphine ligands, leaving one equatorial and two axial carbonyl substituents on the two Ru atoms. The remaining Ru atom carries two equatorial and two axial terminal carbonyl ligands. In the crystal structure, molecules are linked into columns along the a axis by intermolecular C-H...Cl and C-H...O hydrogen bonds. The molecular structure is stabilized by weak intramolecular C-H...O hydrogen bonds.

Comment top

Syntheses and structures of substituted triangulo-triruthenium clusters have been of interest to researchers due to observed structural variations and their potential catalytic activity. As part of our ongoing studies of phosphine substituted triangulo-triruthenium clusters, we report herein the structure of title compound (I).

The asymmetric unit of title compound (I) consists of one triangulo-triruthenium complex and one disordered water solvent (Fig. 1). The geometric parameters of title compound are comparable to those found in a related structure (Chin-Choy et al., 1988). Two monodentate phosphine ligands have replaced carbonyl groups on the Ru1 and Ru2 atoms in the equatorial plane of the Ru3 triangle. The two ligands are approximately trans to the same Ru–Ru bond with P1–Ru1–Ru3 and P2–Ru2–Ru1 bond angles of 166.40 (2) and 167.38 (2)°, respectively. The P1–Ru1–Ru2–P2 torsion angle is 103.95 (14)°. Unlike the monosubsubstituted complexes of the type Ru3(CO)11L [where L = PPh(OMe)2, P(OCH2CF3)3] (Bruce et al., 1988b), there is no pronounced difference in the Ru–Ru separations that can be correlated to the presence of the ligand. The Ru–Ru separations are in the range 2.8517 (3) to 2.8645 (3) Å. The differences in the two Ru–P separations are almost identical with those in the analogous complexes synthesized by Bruce et al. (1988a). In this complex, the equatorial CO groups are more inclined to preserve linearity, equatorial Ru–C–O angles averaging 176.3° while the average value of the axial Ru–C–O groups is 173.8°.

In the crystal structure, the molecules are linked into columns along the a axis by intermolecular C4—H4A···Cl2 and C11—H11A···O8 hydrogen bonds (Fig. 2, Table 1). The molecular structure is stabilized by weak intramolecular C6—H6A···O7 and C24—H24A···O9 hydrogen bonds (Table 1).

Related literature top

For related structures, see: Bruce et al. (1988a,b); Chin-Choy et al. (1988). For the synthesis, see: Bruce et al. (1987). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986).

Experimental top

All the manipulations were performed under a dry oxygen-free nitrogen atmosphere using standard Schlenk techniques. THF was dried over sodium wire and freshly distilled from sodium benzophenone ketyl solution. The title compound (I) was prepared by mixing Ru3(CO)12 (Aldrich) and P(3-Cl-C6H4)3 (Maybridge) in a 1:2 molar ratio in THF at 40 °C. About 0.2 ml of diphenylketyl radical anion initiator (synthesized as per the method of Bruce et al., 1987) was introduced into the reaction mixture under a current of nitrogen. After 20 min. of stirring, the solvent was removed under vacuum. Separation of the product in the pure form was done by preparative thin layer chromatography (mobile phase, dichloromethane: hexane, 1:3) and major red band was separated. Spectroscopic analyses, IR (cyclohexane): ν(CO) 2081, 2059, 2041, 2028, and 2002 cm-1. 1H-NMR (CDCl3, δ); 7.23-7.55 (m, aromatic protons). Single crystals of I (m.p. 159–162° C) were grown by slow diffusion from dichloromethane: methanol at 10 °C

Refinement top

All hydrogen atoms were positioned geometrically and refined using a riding model with C–H = 0.93 Å, Uiso(H) = 1.2 Ueq(C) and O–H = 0.85 Å, Uiso(H) = 1.5 Ueq(O). Two of the 3-chlorophenyl rings (Cl3/C13–C18 and Cl5/C25–C30) are disordered over two positions with refined site-occupancies of 0.671 (3)/0.329 (3) and 0.628 (3)/0.372 (3), respectively. These disordered benzene rings were subjected to rigid bond and similarity restraints. The same Uij parameters were used for the atom pairs C15A/C15B. The water molecule is also disordered over two positions with refined site-occupancies of 0.523 (7) and 0.477 (7). The O atom of the disordered water molecule was refined isotropically. The maximum and minimum residual electron density peaks were located 1.79 Å and 0.39 Å from the H1WA and Cl6 atoms, respectively.

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: 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).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound with 50% probability ellipsoids for non-H atoms.
[Figure 2] Fig. 2. The crystal packing of (I), viewed down the a axis, showing the molecules linked into columns along a axis. Hydrogen atoms not involved in the hydrogen-bonding (dashed lines) and the solvent molecules have been omitted for clarity.
Decacarbonyl-1κ3C,2κ3C,3κ4C-bis[tris(3- chlorophenyl)phosphine]-1κP,2κP-triangulo-triruthenium(0) monohydrate top
Crystal data top
[Ru3(C18H12Cl3P)2(CO)10]·H2OZ = 2
Mr = 1332.52F(000) = 1308
Triclinic, P1Dx = 1.799 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.8063 (1) ÅCell parameters from 9887 reflections
b = 10.9841 (1) Åθ = 2.3–32.5°
c = 21.3087 (2) ŵ = 1.36 mm−1
α = 76.543 (1)°T = 100 K
β = 89.766 (1)°Plate, brown
γ = 89.394 (1)°0.32 × 0.17 × 0.06 mm
V = 2459.71 (4) Å3
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		17915 independent reflections
Radiation source: fine-focus sealed tube13849 reflections with I > 2σ(I)
graphiteRint = 0.037
φ and ω scansθmax = 32.7°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2009)		h = −15→16
Tmin = 0.667, Tmax = 0.919k = −16→16
76122 measured reflectionsl = −32→32
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.044Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.132H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0658P)2 + 3.5923P]
where P = (Fo2 + 2Fc2)/3
17915 reflections(Δ/σ)max = 0.001
735 parametersΔρmax = 3.29 e Å−3
301 restraintsΔρmin = −1.17 e Å−3
Crystal data top
[Ru3(C18H12Cl3P)2(CO)10]·H2Oγ = 89.394 (1)°
Mr = 1332.52V = 2459.71 (4) Å3
Triclinic, P1Z = 2
a = 10.8063 (1) ÅMo Kα radiation
b = 10.9841 (1) ŵ = 1.36 mm−1
c = 21.3087 (2) ÅT = 100 K
α = 76.543 (1)°0.32 × 0.17 × 0.06 mm
β = 89.766 (1)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		17915 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2009)		13849 reflections with I > 2σ(I)
Tmin = 0.667, Tmax = 0.919Rint = 0.037
76122 measured reflectionsθmax = 32.7°
Refinement top
R[F2 > 2σ(F2)] = 0.044H-atom parameters constrained
wR(F2) = 0.132Δρmax = 3.29 e Å−3
S = 1.07Δρmin = −1.17 e Å−3
17915 reflectionsAbsolute structure: ?
735 parametersFlack parameter: ?
301 restraintsRogers parameter: ?
Special details top

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 esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ru10.45268 (2)0.36474 (2)0.214149 (11)0.01749 (5)
Ru20.60936 (2)0.17230 (2)0.286321 (11)0.01872 (6)
Ru30.44475 (2)0.11772 (2)0.191744 (12)0.02019 (6)
Cl10.16663 (12)0.42852 (9)−0.07879 (5)0.0476 (3)
Cl20.14701 (8)0.93629 (7)0.00295 (4)0.02769 (15)
Cl41.13649 (9)−0.06793 (10)0.16900 (5)0.0418 (2)
Cl61.16192 (10)−0.12800 (10)0.47584 (4)0.0423 (2)
P10.28728 (7)0.48755 (7)0.16272 (4)0.01911 (14)
P20.75116 (8)0.00875 (7)0.32315 (4)0.02300 (15)
O10.5710 (2)0.3911 (2)0.08039 (11)0.0309 (5)
O20.6057 (3)0.5704 (3)0.24798 (15)0.0492 (8)
O30.3192 (2)0.3164 (3)0.34537 (11)0.0330 (5)
O40.6561 (3)0.2972 (3)0.39650 (13)0.0413 (7)
O50.8051 (2)0.3200 (2)0.19454 (12)0.0319 (5)
O60.4048 (2)0.0190 (3)0.36790 (12)0.0350 (6)
O70.2023 (2)0.1273 (3)0.26728 (12)0.0308 (5)
O80.3188 (2)0.1585 (3)0.06025 (12)0.0340 (5)
O90.4278 (3)−0.1672 (3)0.22420 (19)0.0513 (9)
O100.6986 (2)0.1230 (2)0.12431 (12)0.0322 (5)
C10.1917 (3)0.4178 (3)0.10969 (15)0.0229 (6)
C20.2085 (3)0.4516 (3)0.04299 (16)0.0264 (6)
H2A0.26380.51430.02470.032*
C30.1416 (4)0.3905 (3)0.00433 (18)0.0319 (7)
C40.0565 (4)0.3000 (3)0.0293 (2)0.0396 (9)
H4A0.01100.26220.00220.048*
C50.0396 (3)0.2659 (3)0.0955 (2)0.0392 (9)
H5A−0.01800.20490.11300.047*
C60.1082 (3)0.3222 (3)0.13611 (19)0.0315 (7)
H6A0.09870.29650.18060.038*
C70.3280 (3)0.6392 (3)0.10949 (14)0.0200 (5)
C80.2342 (3)0.7205 (3)0.08113 (15)0.0219 (5)
H8A0.15180.69930.09010.026*
C90.2634 (3)0.8338 (3)0.03938 (14)0.0220 (5)
C100.3862 (3)0.8684 (3)0.02664 (16)0.0259 (6)
H10A0.40510.9450−0.00080.031*
C110.4792 (3)0.7879 (3)0.05508 (16)0.0280 (6)
H11A0.56150.81000.04670.034*
C120.4506 (3)0.6733 (3)0.09642 (15)0.0240 (6)
H12A0.51400.61940.11540.029*
Cl3A0.2009 (2)0.7404 (2)0.34772 (10)0.0659 (7)0.671 (3)
Cl3B−0.1486 (3)0.5340 (3)0.29616 (17)0.0448 (9)0.329 (3)
C13A0.1723 (8)0.5374 (15)0.2151 (6)0.0208 (15)0.671 (3)
C14A0.2198 (6)0.6039 (10)0.2575 (4)0.0280 (15)0.671 (3)
H14A0.30440.61840.25800.034*0.671 (3)
C15A0.1417 (7)0.6491 (6)0.2994 (3)0.0332 (11)0.671 (3)
C16A0.0163 (7)0.6236 (7)0.3013 (3)0.0423 (15)0.671 (3)
H16A−0.03540.65060.33040.051*0.671 (3)
C17A−0.0308 (6)0.5572 (6)0.2591 (3)0.0378 (13)0.671 (3)
H17A−0.11500.54030.25970.045*0.671 (3)
C18A0.0456 (6)0.5157 (8)0.2160 (4)0.0255 (13)0.671 (3)
H18A0.01200.47280.18740.031*0.671 (3)
C13B0.1952 (15)0.545 (3)0.2260 (12)0.021 (3)0.329 (3)
C18B0.2578 (12)0.6063 (19)0.2661 (9)0.027 (3)0.329 (3)
H18B0.34230.62020.26040.032*0.329 (3)
C17B0.1954 (12)0.6473 (15)0.3147 (7)0.041 (3)0.329 (3)
H17B0.23760.68830.34160.049*0.329 (3)
C16B0.0685 (12)0.6259 (10)0.3225 (6)0.031 (2)0.329 (3)
H16B0.02540.65330.35460.037*0.329 (3)
C15B0.0074 (12)0.5649 (12)0.2831 (6)0.0332 (11)0.329 (3)
C14B0.0683 (12)0.5275 (16)0.2331 (7)0.026 (3)0.329 (3)
H14B0.02460.49140.20470.031*0.329 (3)
C190.8164 (3)−0.0659 (3)0.26168 (15)0.0236 (6)
C200.9393 (3)−0.0454 (3)0.24270 (15)0.0246 (6)
H20A0.9911−0.00110.26400.030*
C210.9835 (3)−0.0919 (3)0.19156 (16)0.0264 (6)
C220.9099 (4)−0.1590 (3)0.15907 (18)0.0329 (7)
H22A0.9420−0.19000.12520.039*
C230.7880 (4)−0.1793 (4)0.1777 (2)0.0389 (9)
H23A0.7368−0.22390.15630.047*
C240.7421 (3)−0.1331 (3)0.2284 (2)0.0364 (8)
H24A0.6599−0.14720.24060.044*
Cl5A0.48872 (18)−0.43467 (14)0.39917 (8)0.0446 (5)0.628 (3)
C25A0.6765 (9)−0.1170 (8)0.3814 (4)0.0241 (18)0.628 (3)
C26A0.6287 (6)−0.2256 (5)0.3696 (2)0.0277 (10)0.628 (3)
H26A0.6469−0.24860.33120.033*0.628 (3)
C27A0.5526 (6)−0.3006 (5)0.4159 (3)0.0318 (11)0.628 (3)
C28A0.5279 (6)−0.2715 (5)0.4748 (3)0.0331 (12)0.628 (3)
H28A0.4780−0.32270.50530.040*0.628 (3)
C29A0.5788 (10)−0.1652 (9)0.4867 (4)0.030 (2)0.628 (3)
H29A0.5655−0.14520.52620.036*0.628 (3)
C30A0.650 (2)−0.0878 (13)0.4403 (7)0.029 (3)0.628 (3)
H30A0.6806−0.01430.44850.035*0.628 (3)
Cl5B0.6595 (4)−0.4829 (2)0.44587 (18)0.0621 (12)0.372 (3)
C25B0.6996 (14)−0.1120 (12)0.3943 (7)0.018 (2)0.372 (3)
C26B0.7019 (10)−0.2373 (8)0.3936 (4)0.0294 (18)0.372 (3)
H26B0.7337−0.26320.35820.035*0.372 (3)
C27B0.6550 (11)−0.3260 (8)0.4475 (5)0.038 (2)0.372 (3)
C28B0.6025 (10)−0.2900 (9)0.4995 (5)0.033 (2)0.372 (3)
H28B0.5672−0.34860.53330.040*0.372 (3)
C29B0.6037 (15)−0.1649 (11)0.5003 (6)0.023 (3)0.372 (3)
H29B0.5700−0.13850.53520.027*0.372 (3)
C30B0.655 (3)−0.0781 (19)0.4491 (11)0.017 (3)0.372 (3)
H30B0.66000.00510.45170.021*0.372 (3)
C310.8909 (3)0.0507 (3)0.36231 (14)0.0247 (6)
C320.9627 (3)−0.0439 (3)0.40081 (15)0.0292 (7)
H32A0.9388−0.12720.40850.035*
C331.0714 (3)−0.0106 (4)0.42754 (15)0.0322 (8)
C341.1090 (3)0.1116 (4)0.41755 (16)0.0334 (7)
H34A1.18120.13140.43650.040*
C351.0381 (3)0.2039 (4)0.37912 (16)0.0307 (7)
H35A1.06300.28680.37140.037*
C360.9292 (3)0.1742 (3)0.35158 (15)0.0267 (6)
H36A0.88180.23750.32580.032*
C370.5301 (3)0.3744 (3)0.13088 (15)0.0228 (6)
C380.5456 (3)0.4933 (3)0.23579 (16)0.0287 (7)
C390.3684 (3)0.3288 (3)0.29689 (15)0.0253 (6)
C400.6417 (3)0.2529 (3)0.35371 (16)0.0266 (6)
C410.7290 (3)0.2659 (3)0.22648 (15)0.0229 (6)
C420.4764 (3)0.0766 (3)0.33450 (15)0.0252 (6)
C430.2945 (3)0.1317 (3)0.24028 (15)0.0255 (6)
C440.3617 (3)0.1470 (3)0.11005 (16)0.0254 (6)
C450.4376 (3)−0.0606 (3)0.21284 (19)0.0321 (7)
C460.6089 (3)0.1238 (3)0.15216 (16)0.0260 (6)
O1W0.8593 (5)0.6098 (5)0.5004 (3)0.0412 (15)*0.523 (7)
H1WA0.81960.60880.46620.062*0.523 (7)
H2WA0.80940.63360.52630.062*0.523 (7)
O2W0.9671 (4)0.5957 (4)0.5008 (2)0.0243 (12)*0.477 (7)
H1WB1.02860.63860.50750.036*0.477 (7)
H2WB0.95040.54400.53610.036*0.477 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01803 (11)0.01647 (10)0.01851 (10)−0.00076 (8)−0.00028 (8)−0.00513 (7)
Ru20.01584 (10)0.01954 (11)0.02046 (10)0.00065 (8)0.00184 (8)−0.00405 (8)
Ru30.01830 (11)0.01931 (11)0.02506 (11)−0.00153 (8)0.00263 (9)−0.00940 (8)
Cl10.0736 (8)0.0353 (5)0.0341 (4)−0.0104 (5)−0.0196 (5)−0.0076 (4)
Cl20.0289 (4)0.0192 (3)0.0330 (4)0.0013 (3)−0.0025 (3)−0.0021 (3)
Cl40.0326 (4)0.0554 (6)0.0471 (5)−0.0144 (4)0.0175 (4)−0.0316 (5)
Cl60.0415 (5)0.0516 (6)0.0298 (4)0.0216 (4)−0.0069 (4)−0.0025 (4)
P10.0188 (3)0.0167 (3)0.0210 (3)−0.0002 (3)0.0027 (3)−0.0028 (3)
P20.0202 (4)0.0214 (3)0.0254 (4)0.0033 (3)0.0049 (3)−0.0018 (3)
O10.0353 (13)0.0298 (12)0.0274 (11)−0.0022 (10)0.0082 (10)−0.0067 (9)
O20.062 (2)0.0402 (16)0.0511 (17)−0.0212 (15)−0.0073 (15)−0.0202 (13)
O30.0331 (13)0.0405 (14)0.0241 (11)0.0031 (11)0.0047 (10)−0.0050 (10)
O40.0386 (15)0.0560 (18)0.0357 (14)0.0077 (13)−0.0037 (12)−0.0242 (13)
O50.0246 (12)0.0399 (14)0.0282 (11)−0.0066 (10)0.0033 (9)−0.0018 (10)
O60.0236 (12)0.0458 (15)0.0303 (12)−0.0030 (11)0.0036 (10)0.0022 (11)
O70.0215 (11)0.0441 (14)0.0294 (11)−0.0022 (10)0.0035 (9)−0.0139 (10)
O80.0283 (12)0.0478 (15)0.0299 (12)−0.0024 (11)0.0008 (10)−0.0175 (11)
O90.0311 (14)0.0237 (13)0.097 (3)−0.0037 (11)0.0019 (16)−0.0097 (15)
O100.0274 (12)0.0356 (13)0.0360 (13)−0.0001 (10)0.0065 (10)−0.0137 (10)
C10.0172 (13)0.0196 (13)0.0303 (14)−0.0015 (10)−0.0037 (11)−0.0025 (11)
C20.0261 (15)0.0199 (13)0.0310 (15)−0.0041 (12)−0.0059 (12)−0.0011 (11)
C30.0373 (19)0.0225 (14)0.0351 (17)−0.0020 (14)−0.0130 (15)−0.0044 (13)
C40.0321 (19)0.0267 (16)0.058 (2)−0.0052 (14)−0.0191 (18)−0.0043 (16)
C50.0213 (16)0.0271 (16)0.065 (3)−0.0073 (13)−0.0088 (17)−0.0022 (17)
C60.0205 (15)0.0264 (15)0.0443 (19)−0.0029 (12)−0.0016 (14)−0.0017 (14)
C70.0220 (13)0.0174 (12)0.0205 (12)−0.0027 (10)0.0022 (10)−0.0040 (10)
C80.0231 (14)0.0168 (12)0.0255 (13)−0.0009 (11)0.0028 (11)−0.0046 (10)
C90.0252 (14)0.0177 (12)0.0232 (13)−0.0001 (11)0.0000 (11)−0.0048 (10)
C100.0289 (16)0.0194 (13)0.0276 (14)−0.0060 (12)0.0011 (12)−0.0015 (11)
C110.0244 (15)0.0250 (15)0.0322 (15)−0.0074 (12)0.0031 (13)−0.0015 (12)
C120.0217 (14)0.0217 (13)0.0279 (14)−0.0037 (11)0.0021 (11)−0.0040 (11)
Cl3A0.0624 (12)0.0899 (15)0.0665 (12)0.0127 (10)−0.0044 (9)−0.0618 (12)
Cl3B0.0233 (13)0.0548 (19)0.059 (2)0.0030 (12)0.0115 (12)−0.0201 (15)
C13A0.023 (3)0.017 (3)0.021 (4)0.001 (3)0.001 (3)−0.003 (2)
C14A0.020 (3)0.032 (3)0.034 (3)−0.001 (3)0.002 (3)−0.012 (2)
C15A0.036 (3)0.034 (3)0.033 (3)0.008 (2)0.003 (2)−0.016 (2)
C16A0.030 (3)0.061 (4)0.040 (3)0.018 (3)0.005 (3)−0.020 (3)
C17A0.027 (3)0.043 (3)0.043 (3)0.006 (2)0.006 (2)−0.011 (3)
C18A0.020 (3)0.026 (3)0.030 (3)0.003 (2)0.000 (2)−0.007 (3)
C13B0.020 (6)0.018 (6)0.025 (9)−0.002 (6)0.006 (6)−0.003 (6)
C18B0.016 (6)0.025 (5)0.046 (8)−0.001 (6)0.007 (6)−0.022 (5)
C17B0.021 (6)0.057 (8)0.053 (8)−0.002 (6)0.007 (6)−0.033 (7)
C16B0.029 (6)0.025 (5)0.042 (7)0.007 (5)0.006 (6)−0.013 (5)
C15B0.036 (3)0.034 (3)0.033 (3)0.008 (2)0.003 (2)−0.016 (2)
C14B0.023 (6)0.028 (6)0.026 (7)−0.001 (5)−0.007 (5)−0.004 (5)
C190.0219 (14)0.0192 (13)0.0296 (14)0.0034 (11)0.0028 (12)−0.0055 (11)
C200.0268 (15)0.0253 (14)0.0221 (13)−0.0013 (12)0.0033 (11)−0.0061 (11)
C210.0251 (15)0.0279 (15)0.0267 (14)−0.0007 (12)0.0040 (12)−0.0071 (12)
C220.0363 (19)0.0311 (17)0.0349 (17)0.0039 (15)−0.0010 (15)−0.0154 (14)
C230.0309 (18)0.0313 (18)0.062 (3)0.0020 (15)−0.0036 (18)−0.0267 (18)
C240.0203 (15)0.0295 (17)0.064 (2)0.0016 (13)0.0010 (16)−0.0195 (17)
Cl5A0.0634 (11)0.0292 (7)0.0399 (8)−0.0127 (7)0.0097 (7)−0.0053 (6)
C25A0.021 (4)0.030 (3)0.020 (3)0.005 (2)0.001 (3)−0.003 (2)
C26A0.035 (3)0.025 (2)0.022 (2)0.008 (2)0.004 (2)−0.0041 (18)
C27A0.040 (3)0.024 (2)0.029 (2)−0.002 (2)0.004 (2)−0.0021 (19)
C28A0.043 (3)0.028 (3)0.025 (2)0.001 (2)0.010 (2)0.0014 (19)
C29A0.036 (5)0.038 (3)0.015 (3)0.004 (3)0.000 (3)−0.003 (2)
C30A0.033 (5)0.033 (4)0.021 (4)0.000 (4)−0.005 (4)−0.005 (3)
Cl5B0.092 (3)0.0191 (11)0.074 (2)−0.0119 (13)0.037 (2)−0.0100 (12)
C25B0.012 (5)0.019 (4)0.023 (6)0.000 (3)−0.001 (4)−0.004 (3)
C26B0.034 (5)0.025 (4)0.030 (4)−0.002 (4)0.008 (4)−0.008 (3)
C27B0.047 (6)0.020 (3)0.047 (5)−0.010 (4)0.022 (5)−0.007 (3)
C28B0.039 (5)0.028 (4)0.032 (4)−0.009 (4)0.010 (4)−0.003 (3)
C29B0.028 (6)0.021 (4)0.018 (6)−0.008 (4)−0.001 (4)−0.002 (3)
C30B0.019 (5)0.020 (4)0.014 (6)−0.005 (4)−0.002 (5)−0.008 (3)
C310.0232 (14)0.0313 (15)0.0190 (12)0.0069 (12)0.0046 (11)−0.0051 (11)
C320.0314 (17)0.0344 (17)0.0206 (13)0.0096 (14)0.0046 (12)−0.0044 (12)
C330.0270 (16)0.047 (2)0.0196 (13)0.0177 (15)0.0001 (12)−0.0037 (13)
C340.0246 (16)0.050 (2)0.0246 (15)0.0071 (15)0.0010 (13)−0.0071 (14)
C350.0239 (15)0.0414 (19)0.0265 (15)0.0022 (14)−0.0003 (12)−0.0071 (13)
C360.0219 (14)0.0328 (16)0.0236 (13)0.0067 (13)0.0020 (11)−0.0034 (12)
C370.0218 (14)0.0211 (13)0.0258 (13)−0.0004 (11)−0.0006 (11)−0.0059 (11)
C380.0321 (17)0.0279 (15)0.0278 (15)−0.0045 (13)−0.0018 (13)−0.0098 (12)
C390.0252 (15)0.0237 (14)0.0258 (14)0.0012 (12)−0.0029 (12)−0.0034 (11)
C400.0205 (14)0.0320 (16)0.0282 (14)0.0038 (12)−0.0014 (12)−0.0092 (12)
C410.0191 (13)0.0265 (14)0.0231 (13)0.0003 (11)−0.0019 (11)−0.0058 (11)
C420.0205 (14)0.0301 (15)0.0226 (13)0.0010 (12)0.0012 (11)−0.0015 (11)
C430.0242 (15)0.0291 (15)0.0249 (13)−0.0002 (12)−0.0010 (12)−0.0099 (12)
C440.0189 (13)0.0277 (15)0.0330 (15)−0.0039 (12)0.0053 (12)−0.0140 (12)
C450.0224 (15)0.0273 (16)0.048 (2)−0.0038 (13)0.0047 (14)−0.0109 (14)
C460.0257 (15)0.0237 (14)0.0305 (15)−0.0015 (12)0.0022 (12)−0.0102 (12)
Geometric parameters (Å, °) top
Ru1—C381.885 (3)C15A—C16A1.385 (10)
Ru1—C371.939 (3)C16A—C17A1.384 (10)
Ru1—C391.940 (3)C16A—H16A0.9300
Ru1—P12.3436 (8)C17A—C18A1.383 (8)
Ru1—Ru22.8517 (3)C17A—H17A0.9300
Ru1—Ru32.8645 (3)C18A—H18A0.9300
Ru2—C401.889 (3)C13B—C14B1.389 (14)
Ru2—C421.934 (3)C13B—C18B1.389 (14)
Ru2—C411.939 (3)C18B—C17B1.391 (13)
Ru2—P22.3423 (8)C18B—H18B0.9300
Ru2—Ru32.8634 (3)C17B—C16B1.397 (14)
Ru3—C451.908 (4)C17B—H17B0.9300
Ru3—C441.920 (3)C16B—C15B1.366 (15)
Ru3—C431.945 (3)C16B—H16B0.9300
Ru3—C461.956 (3)C15B—C14B1.389 (13)
Cl1—C31.743 (4)C14B—H14B0.9300
Cl2—C91.739 (3)C19—C201.392 (4)
Cl4—C211.725 (3)C19—C241.398 (5)
Cl6—C331.745 (4)C20—C211.388 (4)
P1—C13A1.829 (9)C20—H20A0.9300
P1—C11.833 (3)C21—C221.382 (5)
P1—C71.840 (3)C22—C231.380 (5)
P1—C13B1.889 (16)C22—H22A0.9300
P2—C25A1.821 (9)C23—C241.384 (6)
P2—C191.834 (3)C23—H23A0.9300
P2—C311.842 (3)C24—H24A0.9300
P2—C25B1.855 (14)Cl5A—C27A1.743 (6)
O1—C371.137 (4)C25A—C26A1.381 (9)
O2—C381.149 (4)C25A—C30A1.393 (9)
O3—C391.140 (4)C26A—C27A1.399 (7)
O4—C401.141 (4)C26A—H26A0.9300
O5—C411.144 (4)C27A—C28A1.390 (7)
O6—C421.141 (4)C28A—C29A1.372 (9)
O7—C431.145 (4)C28A—H28A0.9300
O8—C441.139 (4)C29A—C30A1.380 (10)
O9—C451.145 (4)C29A—H29A0.9300
O10—C461.136 (4)C30A—H30A0.9300
C1—C21.394 (5)Cl5B—C27B1.731 (8)
C1—C61.406 (4)C25B—C26B1.380 (13)
C2—C31.387 (5)C25B—C30B1.388 (13)
C2—H2A0.9300C26B—C27B1.418 (11)
C3—C41.373 (5)C26B—H26B0.9300
C4—C51.384 (6)C27B—C28B1.380 (11)
C4—H4A0.9300C28B—C29B1.378 (12)
C5—C61.396 (5)C28B—H28B0.9300
C5—H5A0.9300C29B—C30B1.389 (12)
C6—H6A0.9300C29B—H29B0.9300
C7—C81.388 (4)C30B—H30B0.9300
C7—C121.390 (4)C31—C361.389 (5)
C8—C91.389 (4)C31—C321.395 (5)
C8—H8A0.9300C32—C331.396 (5)
C9—C101.392 (4)C32—H32A0.9300
C10—C111.377 (5)C33—C341.374 (6)
C10—H10A0.9300C34—C351.374 (5)
C11—C121.395 (4)C34—H34A0.9300
C11—H11A0.9300C35—C361.392 (5)
C12—H12A0.9300C35—H35A0.9300
Cl3A—C15A1.725 (7)C36—H36A0.9300
Cl3B—C15B1.732 (13)O1W—H1WA0.8499
C13A—C14A1.391 (9)O1W—H2WA0.8500
C13A—C18A1.392 (9)O2W—H1WB0.8499
C14A—C15A1.394 (8)O2W—H2WB0.8501
C14A—H14A0.9300
C38—Ru1—C3796.15 (14)C18A—C17A—C16A121.0 (6)
C38—Ru1—C3992.10 (14)C18A—C17A—H17A119.5
C37—Ru1—C39171.10 (13)C16A—C17A—H17A119.5
C38—Ru1—P198.22 (11)C17A—C18A—C13A120.6 (7)
C37—Ru1—P189.65 (10)C17A—C18A—H18A119.7
C39—Ru1—P192.48 (10)C13A—C18A—H18A119.7
C38—Ru1—Ru293.03 (11)C14B—C13B—C18B119.6 (12)
C37—Ru1—Ru296.75 (9)C14B—C13B—P1122.2 (10)
C39—Ru1—Ru279.43 (10)C18B—C13B—P1118.2 (10)
P1—Ru1—Ru2166.40 (2)C13B—C18B—C17B120.7 (12)
C38—Ru1—Ru3148.79 (11)C13B—C18B—H18B119.7
C37—Ru1—Ru373.58 (9)C17B—C18B—H18B119.7
C39—Ru1—Ru397.60 (10)C18B—C17B—C16B119.0 (11)
P1—Ru1—Ru3110.84 (2)C18B—C17B—H17B120.5
Ru2—Ru1—Ru360.123 (8)C16B—C17B—H17B120.5
C40—Ru2—C4291.90 (14)C15B—C16B—C17B120.1 (10)
C40—Ru2—C4195.74 (14)C15B—C16B—H16B119.9
C42—Ru2—C41171.32 (13)C17B—C16B—H16B119.9
C40—Ru2—P294.52 (10)C16B—C15B—C14B121.1 (11)
C42—Ru2—P291.48 (10)C16B—C15B—Cl3B119.0 (9)
C41—Ru2—P292.00 (10)C14B—C15B—Cl3B119.8 (10)
C40—Ru2—Ru195.96 (10)C15B—C14B—C13B119.3 (12)
C42—Ru2—Ru195.18 (10)C15B—C14B—H14B120.4
C41—Ru2—Ru179.98 (9)C13B—C14B—H14B120.4
P2—Ru2—Ru1167.38 (2)C20—C19—C24118.5 (3)
C40—Ru2—Ru3150.18 (10)C20—C19—P2119.9 (2)
C42—Ru2—Ru374.29 (10)C24—C19—P2121.3 (3)
C41—Ru2—Ru397.03 (9)C21—C20—C19119.1 (3)
P2—Ru2—Ru3111.81 (2)C21—C20—H20A120.5
Ru1—Ru2—Ru360.160 (8)C19—C20—H20A120.5
C45—Ru3—C4497.84 (15)C22—C21—C20122.2 (3)
C45—Ru3—C4392.08 (15)C22—C21—Cl4119.0 (3)
C44—Ru3—C4394.26 (13)C20—C21—Cl4118.8 (3)
C45—Ru3—C4694.45 (14)C23—C22—C21118.9 (3)
C44—Ru3—C4693.01 (14)C23—C22—H22A120.6
C43—Ru3—C46169.48 (13)C21—C22—H22A120.6
C45—Ru3—Ru2103.74 (12)C22—C23—C24119.7 (3)
C44—Ru3—Ru2156.04 (10)C22—C23—H23A120.2
C43—Ru3—Ru295.24 (9)C24—C23—H23A120.2
C46—Ru3—Ru275.20 (10)C23—C24—C19121.7 (3)
C45—Ru3—Ru1157.41 (12)C23—C24—H24A119.2
C44—Ru3—Ru1101.81 (10)C19—C24—H24A119.2
C43—Ru3—Ru175.54 (10)C26A—C25A—C30A118.4 (8)
C46—Ru3—Ru195.52 (9)C26A—C25A—P2126.7 (6)
Ru2—Ru3—Ru159.717 (8)C30A—C25A—P2114.0 (7)
C13A—P1—C1102.7 (3)C25A—C26A—C27A119.4 (6)
C13A—P1—C7100.7 (5)C25A—C26A—H26A120.3
C1—P1—C7102.03 (14)C27A—C26A—H26A120.3
C1—P1—C13B113.5 (5)C28A—C27A—C26A121.7 (5)
C7—P1—C13B99.5 (10)C28A—C27A—Cl5A119.5 (4)
C13A—P1—Ru1116.5 (4)C26A—C27A—Cl5A118.9 (4)
C1—P1—Ru1116.30 (10)C29A—C28A—C27A118.4 (6)
C7—P1—Ru1116.19 (10)C29A—C28A—H28A120.8
C13B—P1—Ru1108.1 (9)C27A—C28A—H28A120.8
C25A—P2—C19105.2 (3)C28A—C29A—C30A120.4 (8)
C25A—P2—C31106.9 (3)C28A—C29A—H29A119.8
C19—P2—C31102.30 (14)C30A—C29A—H29A119.8
C19—P2—C25B110.2 (5)C29A—C30A—C25A121.7 (9)
C31—P2—C25B95.0 (4)C29A—C30A—H30A119.2
C25A—P2—Ru2109.8 (3)C25A—C30A—H30A119.2
C19—P2—Ru2116.10 (11)C26B—C25B—C30B118.4 (12)
C31—P2—Ru2115.63 (11)C26B—C25B—P2120.9 (10)
C25B—P2—Ru2115.1 (5)C30B—C25B—P2120.7 (11)
C2—C1—C6119.2 (3)C25B—C26B—C27B119.2 (9)
C2—C1—P1120.3 (2)C25B—C26B—H26B120.4
C6—C1—P1120.2 (3)C27B—C26B—H26B120.4
C3—C2—C1119.1 (3)C28B—C27B—C26B121.7 (8)
C3—C2—H2A120.5C28B—C27B—Cl5B119.7 (7)
C1—C2—H2A120.5C26B—C27B—Cl5B118.5 (7)
C4—C3—C2122.3 (4)C29B—C28B—C27B118.3 (9)
C4—C3—Cl1118.5 (3)C29B—C28B—H28B120.8
C2—C3—Cl1119.2 (3)C27B—C28B—H28B120.8
C3—C4—C5118.9 (3)C28B—C29B—C30B120.2 (13)
C3—C4—H4A120.6C28B—C29B—H29B119.9
C5—C4—H4A120.6C30B—C29B—H29B119.9
C4—C5—C6120.5 (3)C25B—C30B—C29B121.9 (14)
C4—C5—H5A119.7C25B—C30B—H30B119.0
C6—C5—H5A119.7C29B—C30B—H30B119.0
C5—C6—C1119.9 (4)C36—C31—C32119.5 (3)
C5—C6—H6A120.1C36—C31—P2121.1 (2)
C1—C6—H6A120.1C32—C31—P2119.3 (3)
C8—C7—C12119.3 (3)C31—C32—C33118.4 (3)
C8—C7—P1119.2 (2)C31—C32—H32A120.8
C12—C7—P1121.5 (2)C33—C32—H32A120.8
C7—C8—C9119.9 (3)C34—C33—C32122.3 (3)
C7—C8—H8A120.0C34—C33—Cl6118.9 (3)
C9—C8—H8A120.0C32—C33—Cl6118.8 (3)
C8—C9—C10120.8 (3)C35—C34—C33118.8 (3)
C8—C9—Cl2120.5 (2)C35—C34—H34A120.6
C10—C9—Cl2118.7 (2)C33—C34—H34A120.6
C11—C10—C9119.3 (3)C34—C35—C36120.5 (4)
C11—C10—H10A120.4C34—C35—H35A119.7
C9—C10—H10A120.4C36—C35—H35A119.7
C10—C11—C12120.3 (3)C31—C36—C35120.5 (3)
C10—C11—H11A119.9C31—C36—H36A119.8
C12—C11—H11A119.9C35—C36—H36A119.8
C7—C12—C11120.4 (3)O1—C37—Ru1173.6 (3)
C7—C12—H12A119.8O2—C38—Ru1177.7 (3)
C11—C12—H12A119.8O3—C39—Ru1175.2 (3)
C14A—C13A—C18A118.5 (7)O4—C40—Ru2176.0 (3)
C14A—C13A—P1114.8 (6)O5—C41—Ru2175.4 (3)
C18A—C13A—P1126.7 (6)O6—C42—Ru2173.6 (3)
C13A—C14A—C15A120.6 (7)O7—C43—Ru3172.2 (3)
C13A—C14A—H14A119.7O8—C44—Ru3174.8 (3)
C15A—C14A—H14A119.7O9—C45—Ru3176.7 (3)
C16A—C15A—C14A120.4 (6)O10—C46—Ru3173.0 (3)
C16A—C15A—Cl3A119.7 (5)H1WA—O1W—H2WA107.7
C14A—C15A—Cl3A119.8 (6)H1WA—O1W—H2WB138.0
C17A—C16A—C15A118.9 (5)H2WA—O1W—H2WB107.3
C17A—C16A—H16A120.6H1WB—O2W—H2WB107.7
C15A—C16A—H16A120.6
C38—Ru1—Ru2—C4035.75 (15)C2—C1—C6—C5−2.6 (5)
C37—Ru1—Ru2—C40132.31 (14)P1—C1—C6—C5−177.3 (3)
C39—Ru1—Ru2—C40−55.82 (14)C13A—P1—C7—C8−48.6 (4)
P1—Ru1—Ru2—C40−110.08 (14)C1—P1—C7—C857.0 (3)
Ru3—Ru1—Ru2—C40−161.03 (10)C13B—P1—C7—C8−59.7 (6)
C38—Ru1—Ru2—C42128.22 (15)Ru1—P1—C7—C8−175.4 (2)
C37—Ru1—Ru2—C42−135.22 (13)C13A—P1—C7—C12132.2 (4)
C39—Ru1—Ru2—C4236.65 (14)C1—P1—C7—C12−122.2 (3)
P1—Ru1—Ru2—C42−17.62 (13)C13B—P1—C7—C12121.1 (6)
Ru3—Ru1—Ru2—C42−68.57 (10)Ru1—P1—C7—C125.4 (3)
C38—Ru1—Ru2—C41−59.05 (14)C12—C7—C8—C91.0 (4)
C37—Ru1—Ru2—C4137.51 (13)P1—C7—C8—C9−178.2 (2)
C39—Ru1—Ru2—C41−150.62 (14)C7—C8—C9—C10−1.5 (5)
P1—Ru1—Ru2—C41155.11 (13)C7—C8—C9—Cl2179.5 (2)
Ru3—Ru1—Ru2—C41104.17 (9)C8—C9—C10—C111.1 (5)
C38—Ru1—Ru2—P2−110.22 (15)Cl2—C9—C10—C11−179.9 (3)
C37—Ru1—Ru2—P2−13.66 (14)C9—C10—C11—C12−0.3 (5)
C39—Ru1—Ru2—P2158.21 (14)C8—C7—C12—C11−0.2 (5)
P1—Ru1—Ru2—P2103.95 (14)P1—C7—C12—C11179.0 (3)
Ru3—Ru1—Ru2—P253.00 (11)C10—C11—C12—C7−0.2 (5)
C38—Ru1—Ru2—Ru3−163.22 (11)C1—P1—C13A—C14A−174.9 (10)
C37—Ru1—Ru2—Ru3−66.66 (9)C7—P1—C13A—C14A−69.9 (11)
C39—Ru1—Ru2—Ru3105.21 (10)C13B—P1—C13A—C14A15 (7)
P1—Ru1—Ru2—Ru350.95 (9)Ru1—P1—C13A—C14A56.7 (12)
C40—Ru2—Ru3—C45−122.8 (2)C1—P1—C13A—C18A4.8 (15)
C42—Ru2—Ru3—C45−57.69 (15)C7—P1—C13A—C18A109.9 (13)
C41—Ru2—Ru3—C45122.52 (15)C13B—P1—C13A—C18A−166 (10)
P2—Ru2—Ru3—C4527.51 (11)Ru1—P1—C13A—C18A−123.5 (12)
Ru1—Ru2—Ru3—C45−163.32 (11)C18A—C13A—C14A—C15A−0.8 (19)
C40—Ru2—Ru3—C4483.6 (3)P1—C13A—C14A—C15A178.9 (9)
C42—Ru2—Ru3—C44148.7 (3)C13A—C14A—C15A—C16A2.9 (14)
C41—Ru2—Ru3—C44−31.1 (3)C13A—C14A—C15A—Cl3A−175.6 (10)
P2—Ru2—Ru3—C44−126.1 (2)C14A—C15A—C16A—C17A−2.7 (11)
Ru1—Ru2—Ru3—C4443.1 (2)Cl3A—C15A—C16A—C17A175.8 (5)
C40—Ru2—Ru3—C43−29.3 (2)C15A—C16A—C17A—C18A0.6 (11)
C42—Ru2—Ru3—C4335.75 (14)C16A—C17A—C18A—C13A1.4 (14)
C41—Ru2—Ru3—C43−144.05 (14)C14A—C13A—C18A—C17A−1.3 (18)
P2—Ru2—Ru3—C43120.95 (10)P1—C13A—C18A—C17A179.0 (9)
Ru1—Ru2—Ru3—C43−69.89 (10)C13A—P1—C13B—C14B14 (6)
C40—Ru2—Ru3—C46146.2 (2)C1—P1—C13B—C14B4(3)
C42—Ru2—Ru3—C46−148.73 (14)C7—P1—C13B—C14B111 (3)
C41—Ru2—Ru3—C4631.48 (14)Ru1—P1—C13B—C14B−127 (2)
P2—Ru2—Ru3—C46−63.53 (10)C13A—P1—C13B—C18B−166 (10)
Ru1—Ru2—Ru3—C46105.64 (10)C1—P1—C13B—C18B−176 (2)
C40—Ru2—Ru3—Ru140.5 (2)C7—P1—C13B—C18B−68 (2)
C42—Ru2—Ru3—Ru1105.63 (10)Ru1—P1—C13B—C18B53 (3)
C41—Ru2—Ru3—Ru1−74.16 (10)C14B—C13B—C18B—C17B2(4)
P2—Ru2—Ru3—Ru1−169.16 (2)P1—C13B—C18B—C17B−178.2 (19)
C38—Ru1—Ru3—C4580.4 (3)C13B—C18B—C17B—C16B0(3)
C37—Ru1—Ru3—C45154.6 (3)C18B—C17B—C16B—C15B0(2)
C39—Ru1—Ru3—C45−26.6 (3)C17B—C16B—C15B—C14B−3(2)
P1—Ru1—Ru3—C45−122.2 (3)C17B—C16B—C15B—Cl3B177.3 (11)
Ru2—Ru1—Ru3—C4546.5 (3)C16B—C15B—C14B—C13B5(3)
C38—Ru1—Ru3—C44−129.7 (2)Cl3B—C15B—C14B—C13B−175 (2)
C37—Ru1—Ru3—C44−55.45 (13)C18B—C13B—C14B—C15B−4(4)
C39—Ru1—Ru3—C44123.32 (14)P1—C13B—C14B—C15B176.0 (17)
P1—Ru1—Ru3—C4427.73 (10)C25A—P2—C19—C20−130.3 (4)
Ru2—Ru1—Ru3—C44−163.54 (9)C31—P2—C19—C20−18.7 (3)
C38—Ru1—Ru3—C43138.9 (2)C25B—P2—C19—C20−118.8 (5)
C37—Ru1—Ru3—C43−146.85 (14)Ru2—P2—C19—C20108.1 (3)
C39—Ru1—Ru3—C4331.92 (14)C25A—P2—C19—C2456.3 (4)
P1—Ru1—Ru3—C43−63.67 (10)C31—P2—C19—C24167.8 (3)
Ru2—Ru1—Ru3—C43105.06 (10)C25B—P2—C19—C2467.8 (6)
C38—Ru1—Ru3—C46−35.5 (2)Ru2—P2—C19—C24−65.3 (3)
C37—Ru1—Ru3—C4638.80 (14)C24—C19—C20—C210.2 (5)
C39—Ru1—Ru3—C46−142.43 (14)P2—C19—C20—C21−173.4 (2)
P1—Ru1—Ru3—C46121.98 (10)C19—C20—C21—C22−0.6 (5)
Ru2—Ru1—Ru3—C46−69.29 (10)C19—C20—C21—Cl4−179.2 (2)
C38—Ru1—Ru3—Ru233.8 (2)C20—C21—C22—C230.7 (6)
C37—Ru1—Ru3—Ru2108.09 (10)Cl4—C21—C22—C23179.3 (3)
C39—Ru1—Ru3—Ru2−73.14 (10)C21—C22—C23—C24−0.4 (6)
P1—Ru1—Ru3—Ru2−168.73 (2)C22—C23—C24—C190.0 (6)
C38—Ru1—P1—C13A−77.2 (5)C20—C19—C24—C230.1 (6)
C37—Ru1—P1—C13A−173.4 (5)P2—C19—C24—C23173.6 (3)
C39—Ru1—P1—C13A15.2 (5)C19—P2—C25A—C26A−26.8 (9)
Ru2—Ru1—P1—C13A68.3 (5)C31—P2—C25A—C26A−135.0 (8)
Ru3—Ru1—P1—C13A114.4 (4)C25B—P2—C25A—C26A−143 (4)
C38—Ru1—P1—C1161.40 (16)Ru2—P2—C25A—C26A98.8 (8)
C37—Ru1—P1—C165.24 (15)C19—P2—C25A—C30A163.8 (13)
C39—Ru1—P1—C1−106.12 (15)C31—P2—C25A—C30A55.5 (14)
Ru2—Ru1—P1—C1−53.11 (16)C25B—P2—C25A—C30A47 (4)
Ru3—Ru1—P1—C1−7.02 (12)Ru2—P2—C25A—C30A−70.6 (14)
C38—Ru1—P1—C741.25 (15)C30A—C25A—C26A—C27A1.8 (17)
C37—Ru1—P1—C7−54.91 (14)P2—C25A—C26A—C27A−167.2 (6)
C39—Ru1—P1—C7133.73 (14)C25A—C26A—C27A—C28A−2.7 (10)
Ru2—Ru1—P1—C7−173.26 (11)C25A—C26A—C27A—Cl5A177.9 (6)
Ru3—Ru1—P1—C7−127.17 (10)C26A—C27A—C28A—C29A0.9 (10)
C38—Ru1—P1—C13B−69.5 (8)Cl5A—C27A—C28A—C29A−179.8 (6)
C37—Ru1—P1—C13B−165.7 (8)C27A—C28A—C29A—C30A1.9 (18)
C39—Ru1—P1—C13B23.0 (8)C28A—C29A—C30A—C25A−3(3)
Ru2—Ru1—P1—C13B76.0 (8)C26A—C25A—C30A—C29A1(3)
Ru3—Ru1—P1—C13B122.1 (8)P2—C25A—C30A—C29A171.2 (16)
C40—Ru2—P2—C25A87.4 (3)C25A—P2—C25B—C26B61 (3)
C42—Ru2—P2—C25A−4.7 (3)C19—P2—C25B—C26B−6.2 (12)
C41—Ru2—P2—C25A−176.7 (3)C31—P2—C25B—C26B−111.3 (11)
Ru1—Ru2—P2—C25A−126.6 (3)Ru2—P2—C25B—C26B127.4 (10)
Ru3—Ru2—P2—C25A−78.3 (3)C25A—P2—C25B—C30B−118 (5)
C40—Ru2—P2—C19−153.54 (16)C19—P2—C25B—C30B175 (2)
C42—Ru2—P2—C19114.43 (15)C31—P2—C25B—C30B70 (2)
C41—Ru2—P2—C19−57.62 (15)Ru2—P2—C25B—C30B−51 (2)
Ru1—Ru2—P2—C19−7.48 (18)C30B—C25B—C26B—C27B2(3)
Ru3—Ru2—P2—C1940.77 (12)P2—C25B—C26B—C27B−176.3 (9)
C40—Ru2—P2—C31−33.67 (15)C25B—C26B—C27B—C28B2.7 (18)
C42—Ru2—P2—C31−125.70 (15)C25B—C26B—C27B—Cl5B−179.6 (10)
C41—Ru2—P2—C3162.25 (14)C26B—C27B—C28B—C29B−4.3 (19)
Ru1—Ru2—P2—C31112.39 (14)Cl5B—C27B—C28B—C29B178.0 (10)
Ru3—Ru2—P2—C31160.64 (11)C27B—C28B—C29B—C30B1(3)
C40—Ru2—P2—C25B75.7 (4)C26B—C25B—C30B—C29B−6(4)
C42—Ru2—P2—C25B−16.4 (4)P2—C25B—C30B—C29B173 (2)
C41—Ru2—P2—C25B171.6 (4)C28B—C29B—C30B—C25B4(4)
Ru1—Ru2—P2—C25B−138.3 (4)C25A—P2—C31—C36−143.2 (4)
Ru3—Ru2—P2—C25B−90.0 (4)C19—P2—C31—C36106.5 (3)
C13A—P1—C1—C2130.9 (6)C25B—P2—C31—C36−141.5 (5)
C7—P1—C1—C226.8 (3)Ru2—P2—C31—C36−20.6 (3)
C13B—P1—C1—C2132.9 (12)C25A—P2—C31—C3240.0 (4)
Ru1—P1—C1—C2−100.7 (3)C19—P2—C31—C32−70.3 (3)
C13A—P1—C1—C6−54.5 (6)C25B—P2—C31—C3241.7 (5)
C7—P1—C1—C6−158.5 (3)Ru2—P2—C31—C32162.6 (2)
C13B—P1—C1—C6−52.5 (12)C36—C31—C32—C330.2 (4)
Ru1—P1—C1—C674.0 (3)P2—C31—C32—C33177.0 (2)
C6—C1—C2—C30.4 (5)C31—C32—C33—C340.5 (5)
P1—C1—C2—C3175.1 (3)C31—C32—C33—Cl6179.9 (2)
C1—C2—C3—C41.9 (6)C32—C33—C34—C35−1.0 (5)
C1—C2—C3—Cl1−177.6 (3)Cl6—C33—C34—C35179.5 (3)
C2—C3—C4—C5−2.0 (6)C33—C34—C35—C360.9 (5)
Cl1—C3—C4—C5177.5 (3)C32—C31—C36—C35−0.2 (5)
C3—C4—C5—C6−0.3 (6)P2—C31—C36—C35−177.0 (2)
C4—C5—C6—C12.5 (6)C34—C35—C36—C31−0.3 (5)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C4—H4A···Cl2i0.932.813.607 (4)145
C6—H6A···O70.932.553.259 (5)134
C11—H11A···O8ii0.932.573.234 (4)129
C24—H24A···O90.932.553.425 (5)157
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
C4—H4A···Cl2i0.932.813.607 (4)145
C6—H6A···O70.932.553.259 (5)134
C11—H11A···O8ii0.932.573.234 (4)129
C24—H24A···O90.932.553.425 (5)157
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z.
Acknowledgements top

We gratefully acknowledge funding from the Malaysian Government and Universiti Sains Malaysia (USM) under the University Research Grant 1001/PJJAUH/811115. MAAP thanks USM for a Post-doctoral fellowship, HKF thanks USM for the Research University Golden Goose Grant 1001/PFIZIK/811012 and CSY thanks USM for the award of a USM Fellowship.

references
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