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Acta Crystallogr Sect E Struct Rep Online. 2009 December 1; 65(Pt 12): m1626–m1627.
Published online 2009 November 21. doi:  10.1107/S1600536809047977
PMCID: PMC2972057

[μ-Bis(diphenyl­arsino)methane-1:2κ2 As:As′]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-tricyclo­hexyl­phosphine-3κP-triangulo-triruthenium(0)

Abstract

In the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C18H33P)(CO)9], the bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru3 triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. All three cyclo­hexane rings are disordered over two positions with site occupancies of 0.628 (6) and 0.372 (6). The mean planes of these three phosphine-substituted cyclo­hexane rings make dihedral angles of 53.0 (8), 68.3 (6) and 89.9 (7)° (major components), and 46.7 (14), 41.3 (11) and 75.8 (10)° (minor components) with each other. The dihedral angles between the two phenyl rings are 85.0 (2) and 88.1 (2)° for the two diphenyl­arsino groups. Two cyclo­hexane rings adopt a chair conformation whereas the other adopts a slightly twisted chair conformation for the major components; these conformations are similiar for the minor components. Intra­molecular C—H(...)O hydrogen bonds stabilize the mol­ecular structure. In the crystal packing, the mol­ecules are linked together into chains via inter­molecular C—H(...)O hydrogen bonds down the a axis. Weak inter­molecular C—H(...)π inter­actions further stabilize the crystal structure.

Related literature

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985 [triangle], 1988a [triangle],b [triangle]); Shawkataly et al. (1998 [triangle], 2004 [triangle]). For related structures, see: Shawkataly et al. (2009a [triangle],b [triangle]). For the synthesis of bis­(diphenylarsino)methane, see: Bruce et al. (1983 [triangle]). For ring conformations, see: Cremer & Pople (1975 [triangle]). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-65-m1626-scheme1.jpg

Experimental

Crystal data

  • [Ru3(C25H22As2)(C18H33P)(CO)9]
  • M r = 1307.98
  • Orthorhombic, An external file that holds a picture, illustration, etc.
Object name is e-65-m1626-efi1.jpg
  • a = 15.6489 (2) Å
  • b = 20.9223 (3) Å
  • c = 31.3447 (5) Å
  • V = 10262.6 (3) Å3
  • Z = 8
  • Mo Kα radiation
  • μ = 2.24 mm−1
  • T = 100 K
  • 0.30 × 0.14 × 0.04 mm

Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2005 [triangle]) T min = 0.555, T max = 0.922
  • 62224 measured reflections
  • 11768 independent reflections
  • 8148 reflections with I > 2σ(I)
  • R int = 0.092

Refinement

  • R[F 2 > 2σ(F 2)] = 0.046
  • wR(F 2) = 0.099
  • S = 1.01
  • 11768 reflections
  • 728 parameters
  • 379 restraints
  • H-atom parameters constrained
  • Δρmax = 0.84 e Å−3
  • Δρmin = −0.61 e Å−3

Data collection: APEX2 (Bruker, 2005 [triangle]); cell refinement: SAINT (Bruker, 2005 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009 [triangle]).

Table 1
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809047977/sj2677sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809047977/sj2677Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

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 Postdoctoral Fellowship and to Gokhale Centenary College, Ankola, Karnataka, India, for postdoctoral study leave. HKF thanks USM for the Research University Golden Goose grant 1001/PFIZIK/811012. CSY thanks USM for the award of a USM Fellowship.

supplementary crystallographic information

Comment

Tri-angulotriruthenium clusters are known for their interesting structural variations and related catalytic activity. A large number of substituted derivatives, Ru3(CO)12-nLn (L = group 15 ligand) have been reported (Bruce et al., 1985, 1988a,b). As part of our study on the substitution of transition metal-carbonyl clusters with mixed-ligand complexes, we have published several structures of tri-angulotriruthenium-carbonyl clusters containing mixed P/As and P/Sb ligands (Shawkataly et al., 1998, 2004, 2009a,b). Herein we report the synthesis and structure of Ru3(C18H33P)(C25H22As2)(CO)9.

The bond lengths and angles of title compound (Fig. 1 & 2) are comparable to those in related structures (Shawkataly et al., 2009a,b). The bis(diphenylarsino)methane ligand bridges the Ru1—Ru2 bond and the monodentate phosphine ligand bonds to the Ru3 atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. All three cyclohexane rings are disordered over two positions with site occupancies of 0.628 (6) and 0.372 (6). Only the C41, C42 and C43 atoms in the C38-C43 ring are disordered. The mean planes of these three phosphine-substituted cyclohexane rings make dihedral angles (C26–C31/C32–C37, C26–C31/C38–C43 and C32–C37/C38–C43) of 53.0 (8), 68.3 (6) and 89.9 (7)° with each other respectively for the major components and 46.7 (14), 41.3 (11) and 75.8 (10)° for the minor components. The dihedral angles between the two phenyl rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 85.0 (2) and 88.1 (2)° for the two diphenylarsino groups respectively. Four cyclohexane rings adopt a chair conformation with puckering amplitude Q = 0.555 (17) Å, θ = 0.0 (18)°, [var phi] = 191 (176)° for C26A–C32A ring, Q = 0.572 (18) Å, θ = 180.0 (18)°, [var phi] = 235 (45)° for C32A–C37A ring, Q = 0.52 (3) Å, θ = 10 (3)°, [var phi] = 120 (26)° for C26B–C31B ring and Q = 0.58 (3) Å, θ = 177 (3)°, [var phi] = 90 (166)° for C32B–C37B ring. The other two cyclohexane rings (C38–C43A and C38–C43B) adopt a slightly twisted chair conformation with Q = 0.545 (8) Å, θ = 159.3 (8)°, [var phi] = 137 (2)° and Q = 0.465 (12) Å, θ = 27.0 (14)°, [var phi] = 307 (3)°, respectively (Cremer & Pople, 1975).

In the crystal packing (Fig. 3), intramolecular C31—H31B···O8 and C32—H32A···O9 hydrogen bonds stabilize the molecular structure and the molecules are linked together into chains via intermolecular C43—H43B···O9 hydrogen bonds down a axis. Weak intermolecular C—H···π interactions further stabilize the crystal structure (Table 1).

Experimental

The reactions were conducted under an atmosphere of nitrogen using standard Schlenk techniques and hexane-dried over sodium metal. Tricyclohexylphosphine (Strem Chemicals) used as received and bis(diphenylarsino)methane (Bruce et al., 1983) was prepared by the reported procedure. The title compound was obtained by refluxing equimolar quantities of Ru3(CO)10(µ-Ph2AsCH2AsPh2) (105.5 mg, 0.1 mmol) and tricyclohexylphosphine (27.8 mg, 0.1 mmol) in hexane under nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of CH3OH into CHCl3.

Refinement

All three cyclohexane rings are disordered over two positions. The refined site occupancies are about the same and in the final refinement these site occupancies are made to be the same and refined to 0.628 (6) and 0.372 (6). The same Uij parameters is used for the atom pair C26A/C26B and C32A/C32B. The C26A–C37B atoms were subjected to rigid bond and similarity restraints. All hydrogen atoms were positioned geometrically and refined using a riding model with C—H = 0.93–0.98 Å and Uiso(H) = 1.2 Ueq(C).

Figures

Fig. 1.
The molecular structure of the title compound with 30% probability ellipsoids for non-H atoms. Only the major components are shown.
Fig. 2.
The molecular structure of the title compound with 30% probability ellipsoids for non-H atoms. Only the minor components are shown.
Fig. 3.
The crystal packing of the title compound, viewed down the c axis, showing the molecules linked down a axis. Hydrogen atoms that not involved in the hydrogen-bonding (dashed lines) have been omitted for clarity. Only the major components are shown.

Crystal data

[Ru3(C25H22As2)(C18H33P)(CO)9]F(000) = 5216
Mr = 1307.98Dx = 1.693 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 9061 reflections
a = 15.6489 (2) Åθ = 2.3–26.4°
b = 20.9223 (3) ŵ = 2.24 mm1
c = 31.3447 (5) ÅT = 100 K
V = 10262.6 (3) Å3Plate, red
Z = 80.30 × 0.14 × 0.04 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer11768 independent reflections
Radiation source: fine-focus sealed tube8148 reflections with I > 2σ(I)
graphiteRint = 0.092
[var phi] and ω scansθmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2005)h = −17→20
Tmin = 0.555, Tmax = 0.922k = −27→27
62224 measured reflectionsl = −34→40

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.099H-atom parameters constrained
S = 1.01w = 1/[σ2(Fo2) + (0.0381P)2] where P = (Fo2 + 2Fc2)/3
11768 reflections(Δ/σ)max = 0.001
728 parametersΔρmax = 0.84 e Å3
379 restraintsΔρmin = −0.61 e Å3

Special details

Experimental. The crystal was placed in the cold stream of an Oxford Cyrosystems 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/UeqOcc. (<1)
Ru10.78575 (2)0.257325 (16)0.150385 (12)0.01745 (9)
Ru20.76356 (2)0.392912 (16)0.142057 (12)0.01658 (9)
Ru30.86145 (2)0.324628 (17)0.079835 (12)0.02083 (10)
As10.70760 (3)0.25391 (2)0.216742 (15)0.01608 (11)
As20.65368 (3)0.40103 (2)0.196880 (15)0.01603 (11)
P10.95236 (9)0.26464 (7)0.03344 (4)0.0311 (3)
O10.9585 (2)0.28141 (15)0.19389 (12)0.0305 (8)
O20.8418 (2)0.11900 (15)0.14390 (12)0.0379 (9)
O30.6058 (2)0.24373 (17)0.11196 (12)0.0403 (10)
O40.9075 (2)0.41492 (15)0.20650 (12)0.0336 (9)
O50.7950 (2)0.52994 (15)0.11409 (11)0.0335 (9)
O60.6264 (2)0.37817 (17)0.07316 (12)0.0396 (10)
O71.0200 (3)0.3757 (2)0.12621 (13)0.0594 (13)
O80.8284 (3)0.44135 (18)0.02666 (14)0.0682 (15)
O90.7173 (3)0.2515 (2)0.03533 (14)0.0651 (14)
C10.7736 (3)0.25922 (19)0.26884 (14)0.0165 (10)
C20.7567 (4)0.3011 (2)0.30151 (18)0.0402 (14)
H2A0.71060.32900.29940.048*
C30.8079 (4)0.3022 (3)0.33755 (19)0.0574 (19)
H3A0.79580.33090.35940.069*
C40.8763 (4)0.2614 (3)0.34129 (17)0.0386 (14)
H4A0.91090.26270.36540.046*
C50.8932 (3)0.2191 (2)0.30948 (17)0.0300 (12)
H5A0.93890.19090.31210.036*
C60.8426 (3)0.2176 (2)0.27293 (16)0.0261 (11)
H6A0.85490.18870.25120.031*
C70.6337 (3)0.17998 (19)0.22765 (15)0.0199 (10)
C80.5879 (3)0.1771 (2)0.26535 (16)0.0229 (11)
H8A0.59380.20900.28580.027*
C90.5333 (3)0.1262 (2)0.27232 (17)0.0276 (12)
H9A0.50250.12410.29760.033*
C100.5239 (3)0.0788 (2)0.24239 (18)0.0304 (13)
H10A0.48710.04480.24750.036*
C110.5692 (3)0.0816 (2)0.20470 (17)0.0282 (12)
H11A0.56280.04950.18440.034*
C120.6248 (3)0.1325 (2)0.19694 (16)0.0216 (10)
H12A0.65550.13460.17160.026*
C130.6179 (3)0.31912 (18)0.22109 (15)0.0180 (10)
H13A0.56730.30430.20620.022*
H13B0.60310.32510.25090.022*
C140.5457 (3)0.4367 (2)0.17684 (15)0.0204 (10)
C150.4676 (3)0.4199 (2)0.19500 (16)0.0272 (12)
H15A0.46530.38880.21620.033*
C160.3936 (3)0.4497 (2)0.18139 (18)0.0372 (14)
H16A0.34150.43910.19380.045*
C170.3970 (3)0.4950 (2)0.14949 (17)0.0333 (13)
H17A0.34700.51460.14020.040*
C180.4738 (3)0.5115 (2)0.13144 (16)0.0281 (12)
H18A0.47580.54180.10980.034*
C190.5482 (3)0.4830 (2)0.14539 (15)0.0237 (11)
H19A0.60030.49490.13360.028*
C200.6707 (3)0.45555 (19)0.24663 (15)0.0181 (10)
C210.7242 (3)0.5090 (2)0.24203 (16)0.0235 (11)
H21A0.75430.51540.21680.028*
C220.7318 (3)0.5521 (2)0.27545 (16)0.0268 (12)
H22A0.76710.58760.27250.032*
C230.6874 (3)0.5430 (2)0.31291 (16)0.0260 (11)
H23A0.69280.57230.33500.031*
C240.6351 (3)0.4907 (2)0.31771 (16)0.0274 (11)
H24A0.60590.48440.34320.033*
C250.6257 (3)0.4470 (2)0.28446 (15)0.0212 (10)
H25A0.58940.41210.28760.025*
C26A0.9933 (11)0.3072 (5)−0.0121 (6)0.024 (2)0.628 (6)
H26A1.02980.2778−0.02830.029*0.628 (6)
C27A1.0489 (7)0.3655 (5)0.0017 (4)0.031 (3)0.628 (6)
H27A1.01560.39300.02020.037*0.628 (6)
H27B1.09790.35040.01770.037*0.628 (6)
C28A1.0789 (8)0.4027 (5)−0.0358 (4)0.036 (3)0.628 (6)
H28A1.11740.3763−0.05240.043*0.628 (6)
H28B1.11100.4394−0.02580.043*0.628 (6)
C29A1.0077 (13)0.4257 (6)−0.0644 (6)0.034 (4)0.628 (6)
H29A1.03160.4471−0.08910.041*0.628 (6)
H29B0.97230.4562−0.04910.041*0.628 (6)
C30A0.9523 (14)0.3681 (9)−0.0790 (5)0.022 (3)0.628 (6)
H30A0.90420.3836−0.09550.026*0.628 (6)
H30B0.98620.3406−0.09720.026*0.628 (6)
C31A0.9203 (10)0.3305 (8)−0.0423 (5)0.018 (3)0.628 (6)
H31A0.88920.2937−0.05290.022*0.628 (6)
H31B0.88070.3566−0.02610.022*0.628 (6)
C32A0.8926 (8)0.1935 (6)0.0039 (5)0.025 (2)0.628 (6)
H32A0.83960.2123−0.00710.029*0.628 (6)
C33A0.9359 (8)0.1631 (6)−0.0349 (4)0.033 (3)0.628 (6)
H33A0.95160.1962−0.05520.040*0.628 (6)
H33B0.98780.1415−0.02600.040*0.628 (6)
C34A0.8764 (8)0.1152 (7)−0.0565 (4)0.046 (3)0.628 (6)
H34A0.90560.0961−0.08060.055*0.628 (6)
H34B0.82650.1375−0.06720.055*0.628 (6)
C35A0.8476 (11)0.0620 (7)−0.0259 (6)0.054 (4)0.628 (6)
H35A0.80680.0343−0.04000.065*0.628 (6)
H35B0.89640.0364−0.01730.065*0.628 (6)
C36A0.8073 (14)0.0918 (9)0.0125 (6)0.041 (3)0.628 (6)
H36A0.79260.05840.03260.050*0.628 (6)
H36B0.75460.11270.00390.050*0.628 (6)
C37A0.8636 (17)0.1400 (10)0.0345 (5)0.040 (4)0.628 (6)
H37A0.91350.11850.04600.048*0.628 (6)
H37B0.83260.15880.05820.048*0.628 (6)
C26B0.996 (2)0.3247 (10)−0.0109 (10)0.024 (2)0.372 (6)
H26B1.04530.3027−0.02350.029*0.372 (6)
C27B1.0324 (13)0.3903 (8)0.0049 (7)0.037 (4)0.372 (6)
H27C0.98760.41390.01940.044*0.372 (6)
H27D1.07820.38280.02510.044*0.372 (6)
C28B1.0648 (13)0.4284 (7)−0.0310 (8)0.042 (5)0.372 (6)
H28C1.11220.4057−0.04390.051*0.372 (6)
H28D1.08700.4684−0.01980.051*0.372 (6)
C29B1.000 (2)0.4435 (13)−0.0653 (10)0.042 (5)0.372 (6)
H29C1.02760.4671−0.08820.051*0.372 (6)
H29D0.95480.4696−0.05360.051*0.372 (6)
C30B0.963 (3)0.3795 (17)−0.0826 (9)0.029 (5)0.372 (6)
H30C0.91580.3889−0.10150.034*0.372 (6)
H30D1.00700.3581−0.09930.034*0.372 (6)
C31B0.9339 (19)0.3363 (17)−0.0491 (10)0.033 (6)0.372 (6)
H31C0.92130.2953−0.06210.040*0.372 (6)
H31D0.88080.3530−0.03780.040*0.372 (6)
C32B0.9148 (16)0.2027 (11)0.0066 (9)0.025 (2)0.372 (6)
H32B0.86310.2197−0.00690.029*0.372 (6)
C33B0.9658 (12)0.1758 (11)−0.0309 (8)0.031 (4)0.372 (6)
H33C1.01650.1544−0.02020.037*0.372 (6)
H33D0.98420.2107−0.04910.037*0.372 (6)
C34B0.9128 (13)0.1285 (10)−0.0572 (7)0.036 (4)0.372 (6)
H34C0.94790.1115−0.08000.043*0.372 (6)
H34D0.86520.1510−0.07010.043*0.372 (6)
C35B0.8781 (18)0.0727 (10)−0.0304 (9)0.042 (5)0.372 (6)
H35C0.84130.0459−0.04770.050*0.372 (6)
H35D0.92490.0468−0.01980.050*0.372 (6)
C36B0.828 (2)0.1003 (15)0.0064 (10)0.039 (5)0.372 (6)
H36C0.80800.06580.02440.047*0.372 (6)
H36D0.77870.1229−0.00460.047*0.372 (6)
C37B0.881 (3)0.1458 (16)0.0329 (8)0.033 (5)0.372 (6)
H37C0.92930.12280.04490.040*0.372 (6)
H37D0.84680.16170.05630.040*0.372 (6)
C381.0504 (3)0.2320 (2)0.05776 (16)0.0305 (12)
H38A1.08610.26810.06400.037*0.628 (6)
H38B1.06740.19880.03840.037*0.372 (6)
C391.0385 (3)0.1962 (2)0.09990 (16)0.0276 (12)
H39A1.01050.22400.12030.033*
H39B1.00180.15940.09530.033*
C401.1217 (4)0.1743 (3)0.1179 (2)0.063 (2)
H40A1.10880.14370.13970.075*0.628 (6)
H40B1.14690.21050.13190.075*0.628 (6)
H40C1.12730.13100.10800.075*0.372 (6)
H40D1.11170.17120.14800.075*0.372 (6)
C41A1.1863 (5)0.1466 (5)0.0918 (3)0.041 (3)0.628 (6)
H41A1.17370.10160.08760.050*0.628 (6)
H41B1.24090.14970.10630.050*0.628 (6)
C42A1.1928 (6)0.1786 (5)0.0491 (3)0.050 (3)0.628 (6)
H42A1.22710.15250.03060.060*0.628 (6)
H42B1.22050.21920.05220.060*0.628 (6)
C43A1.1051 (5)0.1885 (4)0.0290 (3)0.040 (2)0.628 (6)
H43A1.07690.14760.02540.048*0.628 (6)
H43B1.11150.20800.00110.048*0.628 (6)
C41B1.1983 (9)0.1995 (7)0.1156 (4)0.033 (4)0.372 (6)
H41C1.24040.16560.11750.039*0.372 (6)
H41D1.20660.22770.13970.039*0.372 (6)
C42B1.2129 (7)0.2360 (6)0.0756 (4)0.024 (3)0.372 (6)
H42C1.22670.20610.05300.029*0.372 (6)
H42D1.26200.26370.07960.029*0.372 (6)
C43B1.1385 (8)0.2757 (7)0.0619 (5)0.034 (4)0.372 (6)
H43C1.15100.29530.03450.041*0.372 (6)
H43D1.12930.30960.08250.041*0.372 (6)
C440.8940 (3)0.2757 (2)0.17588 (16)0.0222 (11)
C450.8187 (3)0.1704 (2)0.14532 (16)0.0249 (11)
C460.6750 (3)0.2500 (2)0.12381 (16)0.0273 (12)
C470.8544 (3)0.4026 (2)0.18272 (16)0.0235 (11)
C480.7813 (3)0.4784 (2)0.12459 (15)0.0227 (11)
C490.6777 (3)0.3804 (2)0.09840 (17)0.0233 (11)
C500.9581 (4)0.3564 (3)0.11070 (17)0.0384 (14)
C510.8451 (4)0.3972 (2)0.04620 (18)0.0370 (14)
C520.7685 (3)0.2794 (3)0.05461 (19)0.0397 (14)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ru10.01512 (19)0.01609 (18)0.0211 (2)0.00056 (15)0.00138 (16)−0.00159 (15)
Ru20.01401 (19)0.01614 (18)0.0196 (2)−0.00059 (14)0.00078 (15)−0.00070 (15)
Ru30.0191 (2)0.02256 (19)0.0208 (2)−0.00073 (16)0.00432 (17)−0.00093 (17)
As10.0128 (2)0.0144 (2)0.0210 (3)0.00013 (18)0.00052 (19)−0.00006 (19)
As20.0130 (2)0.0145 (2)0.0206 (3)−0.00054 (18)0.00109 (19)−0.00064 (19)
P10.0264 (8)0.0408 (8)0.0260 (8)0.0088 (6)0.0061 (6)0.0046 (6)
O10.0181 (19)0.0258 (18)0.048 (2)0.0005 (15)−0.0017 (17)0.0056 (17)
O20.036 (2)0.0181 (18)0.060 (3)0.0037 (16)0.0032 (19)−0.0062 (18)
O30.029 (2)0.048 (2)0.044 (3)−0.0117 (18)−0.0124 (18)0.0036 (19)
O40.028 (2)0.0334 (19)0.039 (2)0.0038 (16)−0.0118 (18)−0.0064 (17)
O50.036 (2)0.0230 (18)0.041 (2)0.0002 (16)0.0156 (17)0.0072 (17)
O60.033 (2)0.047 (2)0.039 (2)0.0095 (18)−0.0193 (19)−0.0144 (19)
O70.035 (3)0.109 (4)0.034 (2)−0.032 (3)0.002 (2)−0.005 (2)
O80.128 (4)0.027 (2)0.050 (3)0.024 (3)0.029 (3)0.011 (2)
O90.043 (3)0.105 (4)0.048 (3)−0.031 (3)0.013 (2)−0.044 (3)
C10.019 (2)0.015 (2)0.015 (2)−0.0028 (18)−0.0008 (19)0.0027 (18)
C20.050 (4)0.035 (3)0.036 (3)0.021 (3)−0.016 (3)−0.008 (3)
C30.089 (5)0.049 (4)0.034 (4)0.032 (4)−0.024 (4)−0.021 (3)
C40.045 (4)0.043 (3)0.028 (3)−0.001 (3)−0.019 (3)0.002 (3)
C50.020 (3)0.031 (3)0.038 (3)0.001 (2)−0.010 (2)0.007 (2)
C60.021 (3)0.028 (3)0.029 (3)0.001 (2)0.001 (2)−0.003 (2)
C70.012 (2)0.015 (2)0.033 (3)0.0018 (18)−0.004 (2)0.004 (2)
C80.021 (3)0.017 (2)0.030 (3)0.001 (2)0.006 (2)0.003 (2)
C90.021 (3)0.024 (3)0.038 (3)−0.001 (2)0.006 (2)0.010 (2)
C100.022 (3)0.019 (2)0.050 (4)−0.006 (2)−0.001 (3)0.006 (2)
C110.021 (3)0.021 (2)0.043 (3)−0.002 (2)−0.006 (2)−0.006 (2)
C120.015 (2)0.021 (2)0.029 (3)0.0001 (19)0.002 (2)0.002 (2)
C130.014 (2)0.016 (2)0.024 (3)−0.0005 (18)0.0002 (19)−0.0007 (19)
C140.019 (3)0.015 (2)0.027 (3)0.0021 (19)−0.001 (2)−0.003 (2)
C150.021 (3)0.029 (3)0.032 (3)0.002 (2)0.004 (2)0.007 (2)
C160.013 (3)0.045 (3)0.054 (4)0.002 (2)0.006 (3)0.009 (3)
C170.027 (3)0.031 (3)0.042 (4)0.008 (2)−0.010 (3)0.001 (3)
C180.031 (3)0.025 (3)0.029 (3)0.002 (2)0.002 (2)0.006 (2)
C190.022 (3)0.016 (2)0.033 (3)0.001 (2)−0.001 (2)0.004 (2)
C200.015 (2)0.015 (2)0.025 (3)0.0032 (18)−0.003 (2)−0.0009 (19)
C210.019 (3)0.024 (2)0.028 (3)−0.001 (2)0.002 (2)−0.001 (2)
C220.020 (3)0.023 (2)0.037 (3)−0.005 (2)−0.002 (2)−0.004 (2)
C230.022 (3)0.029 (3)0.027 (3)0.001 (2)0.000 (2)−0.013 (2)
C240.021 (3)0.034 (3)0.027 (3)0.007 (2)0.007 (2)−0.002 (2)
C250.017 (2)0.016 (2)0.030 (3)0.0016 (19)0.002 (2)−0.001 (2)
C26A0.019 (3)0.024 (6)0.030 (3)0.001 (5)0.012 (2)0.009 (5)
C27A0.018 (5)0.043 (7)0.032 (5)−0.008 (5)−0.002 (4)0.006 (5)
C28A0.034 (6)0.032 (6)0.042 (6)−0.014 (5)−0.007 (4)0.017 (6)
C29A0.036 (7)0.025 (6)0.041 (6)−0.004 (5)0.006 (5)0.013 (5)
C30A0.022 (8)0.022 (7)0.021 (5)0.006 (5)0.002 (5)0.001 (5)
C31A0.011 (5)0.025 (5)0.019 (5)0.004 (4)0.010 (4)0.007 (4)
C32A0.010 (7)0.034 (5)0.029 (4)−0.001 (4)−0.005 (5)−0.007 (3)
C33A0.031 (8)0.038 (7)0.031 (6)0.005 (5)0.005 (6)−0.006 (5)
C34A0.052 (9)0.046 (8)0.040 (6)0.002 (6)−0.006 (6)−0.016 (5)
C35A0.055 (10)0.051 (7)0.056 (8)−0.006 (6)0.000 (7)−0.013 (6)
C36A0.040 (10)0.042 (7)0.042 (7)−0.006 (5)0.004 (6)0.004 (5)
C37A0.042 (11)0.043 (7)0.034 (6)−0.003 (6)0.002 (6)0.008 (5)
C26B0.019 (3)0.024 (6)0.030 (3)0.001 (5)0.012 (2)0.009 (5)
C27B0.024 (9)0.037 (9)0.049 (8)0.013 (7)0.004 (7)−0.019 (7)
C28B0.033 (9)0.018 (8)0.076 (10)−0.012 (8)−0.001 (7)−0.005 (9)
C29B0.025 (10)0.056 (14)0.046 (11)−0.012 (11)0.016 (8)−0.011 (9)
C30B0.018 (10)0.030 (12)0.038 (9)−0.001 (8)0.008 (7)0.016 (7)
C31B0.022 (11)0.039 (11)0.039 (11)−0.006 (8)0.010 (9)−0.009 (8)
C32B0.010 (7)0.034 (5)0.029 (4)−0.001 (4)−0.005 (5)−0.007 (3)
C33B0.017 (10)0.033 (9)0.043 (9)0.000 (7)−0.009 (7)−0.012 (7)
C34B0.035 (12)0.025 (9)0.047 (9)−0.009 (8)0.002 (9)−0.016 (6)
C35B0.069 (16)0.020 (8)0.036 (10)−0.008 (8)0.004 (11)−0.010 (7)
C36B0.032 (14)0.042 (10)0.044 (11)−0.009 (8)−0.001 (8)−0.013 (9)
C37B0.032 (13)0.032 (10)0.036 (10)0.005 (8)−0.007 (8)−0.011 (7)
C380.025 (3)0.039 (3)0.027 (3)0.006 (2)−0.001 (2)0.002 (2)
C390.020 (3)0.037 (3)0.026 (3)−0.004 (2)0.004 (2)−0.003 (2)
C400.042 (4)0.096 (5)0.050 (4)0.007 (4)0.005 (3)0.042 (4)
C41A0.022 (5)0.059 (6)0.043 (6)0.011 (4)−0.001 (4)0.025 (5)
C42A0.037 (6)0.060 (7)0.052 (7)0.004 (5)0.001 (5)0.008 (5)
C43A0.027 (5)0.059 (6)0.034 (5)0.012 (4)−0.004 (4)0.007 (5)
C41B0.037 (9)0.046 (9)0.015 (7)0.015 (7)0.001 (6)0.000 (7)
C42B0.009 (6)0.025 (7)0.039 (9)0.005 (5)0.007 (6)0.000 (6)
C43B0.023 (8)0.042 (8)0.037 (9)−0.010 (6)0.015 (7)0.014 (7)
C440.015 (3)0.021 (2)0.031 (3)0.0038 (19)0.000 (2)0.001 (2)
C450.016 (3)0.029 (3)0.030 (3)−0.005 (2)0.001 (2)−0.002 (2)
C460.026 (3)0.025 (3)0.031 (3)−0.007 (2)−0.007 (2)0.004 (2)
C470.023 (3)0.018 (2)0.029 (3)0.004 (2)0.004 (2)−0.004 (2)
C480.020 (3)0.022 (2)0.025 (3)0.007 (2)0.005 (2)−0.003 (2)
C490.017 (3)0.019 (2)0.034 (3)0.003 (2)0.001 (2)−0.006 (2)
C500.031 (3)0.063 (4)0.021 (3)−0.010 (3)0.010 (3)−0.003 (3)
C510.050 (4)0.027 (3)0.034 (3)0.007 (3)0.010 (3)−0.004 (3)
C520.025 (3)0.053 (4)0.042 (4)−0.006 (3)0.017 (3)−0.019 (3)

Geometric parameters (Å, °)

Ru1—C451.897 (5)C29A—H29B0.9700
Ru1—C441.912 (5)C30A—C31A1.480 (10)
Ru1—C461.930 (5)C30A—H30A0.9700
Ru1—As12.4138 (6)C30A—H30B0.9700
Ru1—Ru22.8699 (5)C31A—H31A0.9700
Ru1—Ru32.8769 (5)C31A—H31B0.9700
Ru2—C481.890 (5)C32A—C33A1.532 (10)
Ru2—C471.920 (5)C32A—C37A1.543 (11)
Ru2—C491.935 (5)C32A—H32A0.9800
Ru2—As22.4369 (6)C33A—C34A1.526 (12)
Ru2—Ru32.8621 (5)C33A—H33A0.9700
Ru3—C511.866 (6)C33A—H33B0.9700
Ru3—C521.906 (6)C34A—C35A1.536 (13)
Ru3—C501.914 (6)C34A—H34A0.9700
Ru3—P12.3905 (14)C34A—H34B0.9700
As1—C11.936 (4)C35A—C36A1.495 (12)
As1—C71.961 (4)C35A—H35A0.9700
As1—C131.962 (4)C35A—H35B0.9700
As2—C201.950 (4)C36A—C37A1.507 (11)
As2—C141.951 (4)C36A—H36A0.9700
As2—C131.956 (4)C36A—H36B0.9700
P1—C32B1.653 (19)C37A—H37A0.9700
P1—C26A1.801 (16)C37A—H37B0.9700
P1—C381.844 (5)C26B—C31B1.561 (15)
P1—C32A1.988 (10)C26B—C27B1.566 (15)
P1—C26B2.00 (3)C26B—H26B0.9800
O1—C441.163 (5)C27B—C28B1.468 (15)
O2—C451.135 (5)C27B—H27C0.9700
O3—C461.151 (5)C27B—H27D0.9700
O4—C471.146 (5)C28B—C29B1.508 (15)
O5—C481.148 (5)C28B—H28C0.9700
O6—C491.128 (5)C28B—H28D0.9700
O7—C501.157 (6)C29B—C30B1.557 (16)
O8—C511.138 (6)C29B—H29C0.9700
O9—C521.161 (6)C29B—H29D0.9700
C1—C21.374 (7)C30B—C31B1.461 (15)
C1—C61.393 (6)C30B—H30C0.9700
C2—C31.385 (8)C30B—H30D0.9700
C2—H2A0.9300C31B—H31C0.9700
C3—C41.375 (7)C31B—H31D0.9700
C3—H3A0.9300C32B—C33B1.530 (15)
C4—C51.359 (7)C32B—C37B1.541 (15)
C4—H4A0.9300C32B—H32B0.9800
C5—C61.393 (7)C33B—C34B1.531 (15)
C5—H5A0.9300C33B—H33C0.9700
C6—H6A0.9300C33B—H33D0.9700
C7—C81.383 (6)C34B—C35B1.537 (15)
C7—C121.390 (6)C34B—H34C0.9700
C8—C91.382 (6)C34B—H34D0.9700
C8—H8A0.9300C35B—C36B1.508 (15)
C9—C101.374 (7)C35B—H35C0.9700
C9—H9A0.9300C35B—H35D0.9700
C10—C111.379 (7)C36B—C37B1.511 (15)
C10—H10A0.9300C36B—H36C0.9700
C11—C121.396 (6)C36B—H36D0.9700
C11—H11A0.9300C37B—H37C0.9700
C12—H12A0.9300C37B—H37D0.9700
C13—H13A0.9700C38—C391.530 (7)
C13—H13B0.9700C38—C43A1.540 (10)
C14—C191.383 (6)C38—C43B1.660 (13)
C14—C151.393 (6)C38—H38A0.9599
C15—C161.382 (6)C38—H38B0.9599
C15—H15A0.9300C39—C401.491 (7)
C16—C171.379 (7)C39—H39A0.9700
C16—H16A0.9300C39—H39B0.9700
C17—C181.373 (7)C40—C41B1.311 (15)
C17—H17A0.9300C40—C41A1.424 (11)
C18—C191.379 (6)C40—H40A0.9601
C18—H18A0.9300C40—H40B0.9601
C19—H19A0.9300C40—H40C0.9599
C20—C251.390 (6)C40—H40D0.9601
C20—C211.404 (6)C41A—C42A1.501 (12)
C21—C221.388 (6)C41A—H40C1.1027
C21—H21A0.9300C41A—H41A0.9700
C22—C231.378 (7)C41A—H41B0.9700
C22—H22A0.9300C42A—C43A1.523 (12)
C23—C241.374 (6)C42A—H42A0.9601
C23—H23A0.9300C42A—H42B0.9600
C24—C251.394 (6)C43A—H38B0.6930
C24—H24A0.9300C43A—H43A0.9700
C25—H25A0.9300C43A—H43B0.9700
C26A—C27A1.559 (10)C41B—C42B1.485 (18)
C26A—C31A1.561 (11)C41B—H40B0.9794
C26A—H26A0.9800C41B—H41C0.9700
C27A—C28A1.486 (10)C41B—H41D0.9700
C27A—H27A0.9700C42B—C43B1.494 (17)
C27A—H27B0.9700C42B—H42B0.8214
C28A—C29A1.509 (11)C42B—H42C0.9700
C28A—H28A0.9700C42B—H42D0.9700
C28A—H28B0.9700C43B—H38A0.8380
C29A—C30A1.554 (10)C43B—H43C0.9700
C29A—H29A0.9700C43B—H43D0.9700
C45—Ru1—C4489.21 (19)C33A—C34A—C35A112.2 (9)
C45—Ru1—C4697.6 (2)C33A—C34A—H34A109.2
C44—Ru1—C46172.98 (19)C35A—C34A—H34A109.2
C45—Ru1—As1100.47 (15)C33A—C34A—H34B109.2
C44—Ru1—As195.42 (15)C35A—C34A—H34B109.2
C46—Ru1—As185.09 (15)H34A—C34A—H34B107.9
C45—Ru1—Ru2166.63 (15)C36A—C35A—C34A108.9 (9)
C44—Ru1—Ru286.96 (13)C36A—C35A—H35A109.9
C46—Ru1—Ru286.03 (14)C34A—C35A—H35A109.9
As1—Ru1—Ru292.653 (17)C36A—C35A—H35B109.9
C45—Ru1—Ru3107.03 (15)C34A—C35A—H35B109.9
C44—Ru1—Ru381.86 (14)H35A—C35A—H35B108.3
C46—Ru1—Ru394.42 (15)C35A—C36A—C37A113.7 (11)
As1—Ru1—Ru3152.304 (19)C35A—C36A—H36A108.8
Ru2—Ru1—Ru359.741 (12)C37A—C36A—H36A108.8
C48—Ru2—C4789.1 (2)C35A—C36A—H36B108.8
C48—Ru2—C4991.4 (2)C37A—C36A—H36B108.8
C47—Ru2—C49176.01 (19)H36A—C36A—H36B107.7
C48—Ru2—As2103.99 (14)C36A—C37A—C32A111.8 (9)
C47—Ru2—As292.68 (14)C36A—C37A—H37A109.3
C49—Ru2—As291.05 (14)C32A—C37A—H37A109.3
C48—Ru2—Ru3101.32 (14)C36A—C37A—H37B109.3
C47—Ru2—Ru396.26 (13)C32A—C37A—H37B109.3
C49—Ru2—Ru379.76 (13)H37A—C37A—H37B107.9
As2—Ru2—Ru3153.251 (19)C31B—C26B—C27B109.4 (15)
C48—Ru2—Ru1160.66 (13)C31B—C26B—P1114.7 (17)
C47—Ru2—Ru187.40 (13)C27B—C26B—P1117.1 (18)
C49—Ru2—Ru190.85 (13)C31B—C26B—H26B104.7
As2—Ru2—Ru195.171 (17)C27B—C26B—H26B104.7
Ru3—Ru2—Ru160.251 (13)P1—C26B—H26B104.7
C51—Ru3—C5293.7 (3)C28B—C27B—C26B111.1 (14)
C51—Ru3—C5096.4 (2)C28B—C27B—H27C109.4
C52—Ru3—C50169.9 (3)C26B—C27B—H27C109.4
C51—Ru3—P199.51 (16)C28B—C27B—H27D109.4
C52—Ru3—P186.64 (16)C26B—C27B—H27D109.4
C50—Ru3—P191.13 (17)H27C—C27B—H27D108.0
C51—Ru3—Ru284.57 (16)C27B—C28B—C29B115.3 (15)
C52—Ru3—Ru297.00 (15)C27B—C28B—H28C108.4
C50—Ru3—Ru284.55 (16)C29B—C28B—H28C108.4
P1—Ru3—Ru2174.39 (4)C27B—C28B—H28D108.4
C51—Ru3—Ru1140.89 (16)C29B—C28B—H28D108.4
C52—Ru3—Ru176.23 (18)H28C—C28B—H28D107.5
C50—Ru3—Ru196.13 (16)C28B—C29B—C30B108.6 (16)
P1—Ru3—Ru1117.11 (4)C28B—C29B—H29C110.0
Ru2—Ru3—Ru160.008 (12)C30B—C29B—H29C110.0
C1—As1—C7102.29 (18)C28B—C29B—H29D110.0
C1—As1—C13106.47 (19)C30B—C29B—H29D110.0
C7—As1—C1396.59 (17)H29C—C29B—H29D108.4
C1—As1—Ru1117.05 (13)C31B—C30B—C29B113.5 (18)
C7—As1—Ru1118.18 (14)C31B—C30B—H30C108.9
C13—As1—Ru1113.68 (13)C29B—C30B—H30C108.9
C20—As2—C1498.75 (18)C31B—C30B—H30D108.9
C20—As2—C13103.96 (18)C29B—C30B—H30D108.9
C14—As2—C13102.23 (18)H30C—C30B—H30D107.7
C20—As2—Ru2120.55 (13)C30B—C31B—C26B116.8 (16)
C14—As2—Ru2114.26 (14)C30B—C31B—H31C108.1
C13—As2—Ru2114.48 (13)C26B—C31B—H31C108.1
C32B—P1—C26A96.3 (11)C30B—C31B—H31D108.1
C32B—P1—C38102.5 (11)C26B—C31B—H31D108.1
C26A—P1—C38102.4 (6)H31C—C31B—H31D107.3
C26A—P1—C32A99.7 (6)C33B—C32B—C37B107.7 (15)
C38—P1—C32A107.9 (5)C33B—C32B—P1119.6 (14)
C32B—P1—C26B105.1 (12)C37B—C32B—P1117.1 (18)
C38—P1—C26B103.7 (10)C33B—C32B—H32B103.3
C32A—P1—C26B107.9 (9)C37B—C32B—H32B103.3
C32B—P1—Ru3120.6 (8)P1—C32B—H32B103.3
C26A—P1—Ru3115.8 (5)C32B—C33B—C34B111.6 (13)
C38—P1—Ru3115.98 (18)C32B—C33B—H33C109.3
C32A—P1—Ru3113.4 (4)C34B—C33B—H33C109.3
C26B—P1—Ru3107.3 (10)C32B—C33B—H33D109.3
C2—C1—C6118.7 (4)C34B—C33B—H33D109.3
C2—C1—As1124.2 (4)H33C—C33B—H33D108.0
C6—C1—As1117.1 (3)C33B—C34B—C35B112.9 (13)
C1—C2—C3120.5 (5)C33B—C34B—H34C109.0
C1—C2—H2A119.8C35B—C34B—H34C109.0
C3—C2—H2A119.8C33B—C34B—H34D109.0
C4—C3—C2120.6 (5)C35B—C34B—H34D109.0
C4—C3—H3A119.7H34C—C34B—H34D107.8
C2—C3—H3A119.7C36B—C35B—C34B108.0 (13)
C5—C4—C3119.6 (5)C36B—C35B—H35C110.1
C5—C4—H4A120.2C34B—C35B—H35C110.1
C3—C4—H4A120.2C36B—C35B—H35D110.1
C4—C5—C6120.5 (5)C34B—C35B—H35D110.1
C4—C5—H5A119.8H35C—C35B—H35D108.4
C6—C5—H5A119.8C35B—C36B—C37B112.2 (17)
C1—C6—C5120.1 (5)C35B—C36B—H36C109.2
C1—C6—H6A119.9C37B—C36B—H36C109.2
C5—C6—H6A119.9C35B—C36B—H36D109.2
C8—C7—C12120.5 (4)C37B—C36B—H36D109.2
C8—C7—As1119.3 (3)H36C—C36B—H36D107.9
C12—C7—As1120.1 (4)C36B—C37B—C32B112.3 (15)
C9—C8—C7119.3 (5)C36B—C37B—H37C109.1
C9—C8—H8A120.4C32B—C37B—H37C109.1
C7—C8—H8A120.4C36B—C37B—H37D109.1
C10—C9—C8121.0 (5)C32B—C37B—H37D109.1
C10—C9—H9A119.5H37C—C37B—H37D107.9
C8—C9—H9A119.5C39—C38—C43A106.5 (5)
C9—C10—C11119.9 (4)C39—C38—C43B107.7 (6)
C9—C10—H10A120.0C43A—C38—C43B84.8 (7)
C11—C10—H10A120.0C39—C38—P1115.9 (3)
C10—C11—C12120.1 (5)C43A—C38—P1116.0 (4)
C10—C11—H11A119.9C43B—C38—P1121.2 (6)
C12—C11—H11A119.9C39—C38—H38A106.2
C7—C12—C11119.1 (5)C43A—C38—H38A105.1
C7—C12—H12A120.4P1—C38—H38A106.1
C11—C12—H12A120.4C39—C38—H38B103.1
As2—C13—As1112.2 (2)C43B—C38—H38B102.5
As2—C13—H13A109.2P1—C38—H38B103.7
As1—C13—H13A109.2H38A—C38—H38B122.4
As2—C13—H13B109.2C40—C39—C38111.7 (4)
As1—C13—H13B109.2C40—C39—H39A109.3
H13A—C13—H13B107.9C38—C39—H39A109.3
C19—C14—C15119.5 (4)C40—C39—H39B109.3
C19—C14—As2118.2 (3)C38—C39—H39B109.3
C15—C14—As2122.1 (4)H39A—C39—H39B107.9
C16—C15—C14119.7 (5)C41B—C40—C41A58.9 (7)
C16—C15—H15A120.2C41B—C40—C39130.9 (8)
C14—C15—H15A120.2C41A—C40—C39121.9 (6)
C17—C16—C15120.1 (5)C41B—C40—H40A120.0
C17—C16—H16A119.9C41A—C40—H40A106.7
C15—C16—H16A119.9C39—C40—H40A106.9
C18—C17—C16120.3 (5)C41B—C40—H40B48.1
C18—C17—H17A119.9C41A—C40—H40B107.0
C16—C17—H17A119.9C39—C40—H40B106.8
C17—C18—C19120.0 (5)H40A—C40—H40B106.6
C17—C18—H18A120.0C41B—C40—H40C106.1
C19—C18—H18A120.0C41A—C40—H40C50.7
C18—C19—C14120.3 (4)C39—C40—H40C104.4
C18—C19—H19A119.8H40A—C40—H40C67.7
C14—C19—H19A119.8H40B—C40—H40C148.5
C25—C20—C21119.5 (4)C41B—C40—H40D103.3
C25—C20—As2122.5 (3)C41A—C40—H40D130.9
C21—C20—As2117.7 (3)C39—C40—H40D104.5
C22—C21—C20119.4 (4)H40B—C40—H40D70.7
C22—C21—H21A120.3H40C—C40—H40D105.6
C20—C21—H21A120.3C40—C41A—C42A112.2 (7)
C23—C22—C21120.6 (4)C42A—C41A—H40C126.9
C23—C22—H22A119.7C40—C41A—H41A109.2
C21—C22—H22A119.7C42A—C41A—H41A109.2
C24—C23—C22120.3 (4)H40C—C41A—H41A66.8
C24—C23—H23A119.9C40—C41A—H41B109.2
C22—C23—H23A119.9C42A—C41A—H41B109.2
C23—C24—C25120.2 (4)H40C—C41A—H41B122.7
C23—C24—H24A119.9H41A—C41A—H41B107.9
C25—C24—H24A119.9C41A—C42A—C43A111.6 (8)
C20—C25—C24120.0 (4)C41A—C42A—H42A108.8
C20—C25—H25A120.0C43A—C42A—H42A109.4
C24—C25—H25A120.0C41A—C42A—H42B109.6
C27A—C26A—C31A109.4 (8)C43A—C42A—H42B109.2
C27A—C26A—P1111.4 (10)H42A—C42A—H42B108.2
C31A—C26A—P1112.0 (11)C42A—C43A—C38109.8 (7)
C27A—C26A—H26A108.0C42A—C43A—H38B129.2
C31A—C26A—H26A108.0C42A—C43A—H43A109.7
P1—C26A—H26A108.0C38—C43A—H43A109.7
C28A—C27A—C26A111.5 (8)H38B—C43A—H43A86.4
C28A—C27A—H27A109.3C42A—C43A—H43B109.7
C26A—C27A—H27A109.3C38—C43A—H43B109.7
C28A—C27A—H27B109.3H38B—C43A—H43B109.9
C26A—C27A—H27B109.3H43A—C43A—H43B108.2
H27A—C27A—H27B108.0C40—C41B—C42B113.2 (11)
C27A—C28A—C29A113.8 (9)C40—C41B—H40B46.9
C27A—C28A—H28A108.8C42B—C41B—H40B116.4
C29A—C28A—H28A108.8C40—C41B—H41C108.9
C27A—C28A—H28B108.8C42B—C41B—H41C108.9
C29A—C28A—H28B108.8H40B—C41B—H41C134.1
H28A—C28A—H28B107.7C40—C41B—H41D108.9
C28A—C29A—C30A109.7 (9)C42B—C41B—H41D108.9
C28A—C29A—H29A109.7H40B—C41B—H41D63.8
C30A—C29A—H29A109.7H41C—C41B—H41D107.8
C28A—C29A—H29B109.7C41B—C42B—C43B114.1 (11)
C30A—C29A—H29B109.7C41B—C42B—H42B123.8
H29A—C29A—H29B108.2C43B—C42B—H42B95.3
C31A—C30A—C29A111.9 (9)C41B—C42B—H42C108.7
C31A—C30A—H30A109.2C43B—C42B—H42C108.7
C29A—C30A—H30A109.2C41B—C42B—H42D108.7
C31A—C30A—H30B109.2C43B—C42B—H42D108.7
C29A—C30A—H30B109.2H42B—C42B—H42D104.8
H30A—C30A—H30B107.9H42C—C42B—H42D107.6
C30A—C31A—C26A112.9 (11)C42B—C43B—C38111.3 (10)
C30A—C31A—H31A109.0C42B—C43B—H38A129.2
C26A—C31A—H31A109.0C42B—C43B—H43C109.4
C30A—C31A—H31B109.0C38—C43B—H43C109.4
C26A—C31A—H31B109.0H38A—C43B—H43C110.5
H31A—C31A—H31B107.8C42B—C43B—H43D109.4
C33A—C32A—C37A108.9 (9)C38—C43B—H43D109.4
C33A—C32A—P1118.2 (7)H38A—C43B—H43D86.6
C37A—C32A—P1113.0 (10)H43C—C43B—H43D108.0
C33A—C32A—H32A105.2O1—C44—Ru1173.2 (4)
C37A—C32A—H32A105.2O2—C45—Ru1176.3 (4)
P1—C32A—H32A105.2O3—C46—Ru1173.0 (5)
C34A—C33A—C32A110.7 (8)O4—C47—Ru2173.1 (4)
C34A—C33A—H33A109.5O5—C48—Ru2177.7 (4)
C32A—C33A—H33A109.5O6—C49—Ru2174.5 (4)
C34A—C33A—H33B109.5O7—C50—Ru3174.4 (5)
C32A—C33A—H33B109.5O8—C51—Ru3174.5 (5)
H33A—C33A—H33B108.1O9—C52—Ru3172.6 (5)
C45—Ru1—Ru2—C48−10.2 (8)As1—C7—C12—C11−177.5 (3)
C44—Ru1—Ru2—C4863.3 (5)C10—C11—C12—C70.0 (7)
C46—Ru1—Ru2—C48−116.5 (5)C20—As2—C13—As1−107.7 (2)
As1—Ru1—Ru2—C48158.6 (4)C14—As2—C13—As1149.9 (2)
Ru3—Ru1—Ru2—C48−19.0 (4)Ru2—As2—C13—As125.8 (3)
C45—Ru1—Ru2—C47−89.9 (6)C1—As1—C13—As291.1 (2)
C44—Ru1—Ru2—C47−16.4 (2)C7—As1—C13—As2−164.0 (2)
C46—Ru1—Ru2—C47163.8 (2)Ru1—As1—C13—As2−39.2 (2)
As1—Ru1—Ru2—C4778.91 (14)C20—As2—C14—C1995.6 (4)
Ru3—Ru1—Ru2—C47−98.73 (14)C13—As2—C14—C19−158.0 (4)
C45—Ru1—Ru2—C4986.5 (6)Ru2—As2—C14—C19−33.7 (4)
C44—Ru1—Ru2—C49160.0 (2)C20—As2—C14—C15−80.3 (4)
C46—Ru1—Ru2—C49−19.8 (2)C13—As2—C14—C1526.1 (4)
As1—Ru1—Ru2—C49−104.67 (14)Ru2—As2—C14—C15150.4 (3)
Ru3—Ru1—Ru2—C4977.69 (14)C19—C14—C15—C160.0 (7)
C45—Ru1—Ru2—As2177.6 (6)As2—C14—C15—C16175.8 (4)
C44—Ru1—Ru2—As2−108.84 (15)C14—C15—C16—C171.1 (8)
C46—Ru1—Ru2—As271.35 (16)C15—C16—C17—C18−0.8 (8)
As1—Ru1—Ru2—As2−13.54 (2)C16—C17—C18—C19−0.5 (8)
Ru3—Ru1—Ru2—As2168.818 (19)C17—C18—C19—C141.5 (7)
C45—Ru1—Ru2—Ru38.8 (6)C15—C14—C19—C18−1.3 (7)
C44—Ru1—Ru2—Ru382.35 (15)As2—C14—C19—C18−177.3 (4)
C46—Ru1—Ru2—Ru3−97.47 (16)C14—As2—C20—C2576.4 (4)
As1—Ru1—Ru2—Ru3177.639 (19)C13—As2—C20—C25−28.6 (4)
C48—Ru2—Ru3—C51−23.6 (2)Ru2—As2—C20—C25−158.6 (3)
C47—Ru2—Ru3—C51−113.9 (2)C14—As2—C20—C21−97.1 (4)
C49—Ru2—Ru3—C5165.8 (2)C13—As2—C20—C21157.8 (3)
As2—Ru2—Ru3—C51137.30 (18)Ru2—As2—C20—C2127.9 (4)
Ru1—Ru2—Ru3—C51162.72 (18)C25—C20—C21—C220.4 (6)
C48—Ru2—Ru3—C52−116.7 (2)As2—C20—C21—C22174.2 (3)
C47—Ru2—Ru3—C52153.0 (2)C20—C21—C22—C230.0 (7)
C49—Ru2—Ru3—C52−27.3 (2)C21—C22—C23—C240.2 (7)
As2—Ru2—Ru3—C5244.2 (2)C22—C23—C24—C25−0.9 (7)
Ru1—Ru2—Ru3—C5269.65 (19)C21—C20—C25—C24−1.1 (6)
C48—Ru2—Ru3—C5073.4 (2)As2—C20—C25—C24−174.5 (3)
C47—Ru2—Ru3—C50−16.9 (2)C23—C24—C25—C201.3 (7)
C49—Ru2—Ru3—C50162.8 (2)C32B—P1—C26A—C27A−170.5 (14)
As2—Ru2—Ru3—C50−125.72 (18)C38—P1—C26A—C27A−66.2 (11)
Ru1—Ru2—Ru3—C50−100.31 (17)C32A—P1—C26A—C27A−177.0 (10)
C48—Ru2—Ru3—Ru1173.68 (15)C26B—P1—C26A—C27A32 (8)
C47—Ru2—Ru3—Ru183.38 (14)Ru3—P1—C26A—C27A61.0 (11)
C49—Ru2—Ru3—Ru1−96.93 (14)C32B—P1—C26A—C31A66.7 (15)
As2—Ru2—Ru3—Ru1−25.41 (4)C38—P1—C26A—C31A171.0 (10)
C45—Ru1—Ru3—C51154.2 (3)C32A—P1—C26A—C31A60.1 (11)
C44—Ru1—Ru3—C51−119.2 (3)C26B—P1—C26A—C31A−90 (9)
C46—Ru1—Ru3—C5154.8 (3)Ru3—P1—C26A—C31A−61.8 (11)
As1—Ru1—Ru3—C51−33.0 (3)C31A—C26A—C27A—C28A−52.6 (16)
Ru2—Ru1—Ru3—C51−28.0 (3)P1—C26A—C27A—C28A−176.9 (9)
C45—Ru1—Ru3—C5275.5 (2)C26A—C27A—C28A—C29A56.1 (14)
C44—Ru1—Ru3—C52162.1 (2)C27A—C28A—C29A—C30A−55.5 (17)
C46—Ru1—Ru3—C52−23.9 (2)C28A—C29A—C30A—C31A54.5 (19)
As1—Ru1—Ru3—C52−111.72 (17)C29A—C30A—C31A—C26A−55.2 (18)
Ru2—Ru1—Ru3—C52−106.64 (17)C27A—C26A—C31A—C30A53.5 (17)
C45—Ru1—Ru3—C50−97.8 (2)P1—C26A—C31A—C30A177.5 (11)
C44—Ru1—Ru3—C50−11.1 (2)C32B—P1—C32A—C33A−23 (11)
C46—Ru1—Ru3—C50162.9 (2)C26A—P1—C32A—C33A40.4 (12)
As1—Ru1—Ru3—C5075.00 (18)C38—P1—C32A—C33A−66.1 (11)
Ru2—Ru1—Ru3—C5080.08 (18)C26B—P1—C32A—C33A45.3 (16)
C45—Ru1—Ru3—P1−3.37 (16)Ru3—P1—C32A—C33A164.0 (9)
C44—Ru1—Ru3—P183.29 (14)C32B—P1—C32A—C37A106 (12)
C46—Ru1—Ru3—P1−102.70 (15)C26A—P1—C32A—C37A169.2 (13)
As1—Ru1—Ru3—P1169.44 (5)C38—P1—C32A—C37A62.7 (12)
Ru2—Ru1—Ru3—P1174.52 (4)C26B—P1—C32A—C37A174.1 (16)
C45—Ru1—Ru3—Ru2−177.88 (15)Ru3—P1—C32A—C37A−67.1 (12)
C44—Ru1—Ru3—Ru2−91.23 (13)C37A—C32A—C33A—C34A56.0 (14)
C46—Ru1—Ru3—Ru282.79 (15)P1—C32A—C33A—C34A−173.2 (10)
As1—Ru1—Ru3—Ru2−5.08 (4)C32A—C33A—C34A—C35A−58.0 (14)
C45—Ru1—As1—C183.3 (2)C33A—C34A—C35A—C36A55.6 (15)
C44—Ru1—As1—C1−6.90 (19)C34A—C35A—C36A—C37A−54.7 (18)
C46—Ru1—As1—C1−179.88 (19)C35A—C36A—C37A—C32A56 (2)
Ru2—Ru1—As1—C1−94.10 (14)C33A—C32A—C37A—C36A−55.0 (17)
Ru3—Ru1—As1—C1−89.71 (14)P1—C32A—C37A—C36A171.4 (13)
C45—Ru1—As1—C7−39.7 (2)C32B—P1—C26B—C31B47 (3)
C44—Ru1—As1—C7−129.91 (19)C26A—P1—C26B—C31B70 (8)
C46—Ru1—As1—C757.1 (2)C38—P1—C26B—C31B154 (2)
Ru2—Ru1—As1—C7142.90 (14)C32A—P1—C26B—C31B40 (2)
Ru3—Ru1—As1—C7147.29 (14)Ru3—P1—C26B—C31B−83 (2)
C45—Ru1—As1—C13−151.9 (2)C32B—P1—C26B—C27B177 (2)
C44—Ru1—As1—C13117.94 (19)C26A—P1—C26B—C27B−159 (10)
C46—Ru1—As1—C13−55.03 (19)C38—P1—C26B—C27B−76 (2)
Ru2—Ru1—As1—C1330.75 (14)C32A—P1—C26B—C27B170.2 (17)
Ru3—Ru1—As1—C1335.14 (14)Ru3—P1—C26B—C27B48 (2)
C48—Ru2—As2—C20−56.2 (2)C31B—C26B—C27B—C28B−49 (3)
C47—Ru2—As2—C2033.48 (19)P1—C26B—C27B—C28B178.0 (17)
C49—Ru2—As2—C20−147.95 (19)C26B—C27B—C28B—C29B59 (2)
Ru3—Ru2—As2—C20143.07 (14)C27B—C28B—C29B—C30B−57 (3)
Ru1—Ru2—As2—C20121.11 (14)C28B—C29B—C30B—C31B50 (4)
C48—Ru2—As2—C1461.1 (2)C29B—C30B—C31B—C26B−48 (4)
C47—Ru2—As2—C14150.85 (19)C27B—C26B—C31B—C30B47 (4)
C49—Ru2—As2—C14−30.57 (19)P1—C26B—C31B—C30B−180 (3)
Ru3—Ru2—As2—C14−99.56 (14)C26A—P1—C32B—C33B39 (2)
Ru1—Ru2—As2—C14−121.52 (14)C38—P1—C32B—C33B−65 (2)
C48—Ru2—As2—C13178.6 (2)C32A—P1—C32B—C33B157 (14)
C47—Ru2—As2—C13−91.73 (19)C26B—P1—C32B—C33B43 (2)
C49—Ru2—As2—C1386.8 (2)Ru3—P1—C32B—C33B164.3 (16)
Ru3—Ru2—As2—C1317.87 (16)C26A—P1—C32B—C37B172 (2)
Ru1—Ru2—As2—C13−4.10 (15)C38—P1—C32B—C37B68 (2)
C51—Ru3—P1—C32B−104.8 (13)C32A—P1—C32B—C37B−70 (12)
C52—Ru3—P1—C32B−11.6 (13)C26B—P1—C32B—C37B176 (2)
C50—Ru3—P1—C32B158.5 (13)Ru3—P1—C32B—C37B−62 (2)
Ru1—Ru3—P1—C32B61.0 (13)C37B—C32B—C33B—C34B55 (2)
C51—Ru3—P1—C26A10.5 (5)P1—C32B—C33B—C34B−168 (2)
C52—Ru3—P1—C26A103.7 (5)C32B—C33B—C34B—C35B−57 (2)
C50—Ru3—P1—C26A−86.1 (5)C33B—C34B—C35B—C36B55 (2)
Ru1—Ru3—P1—C26A176.4 (5)C34B—C35B—C36B—C37B−56 (3)
C51—Ru3—P1—C38130.6 (3)C35B—C36B—C37B—C32B60 (3)
C52—Ru3—P1—C38−136.2 (3)C33B—C32B—C37B—C36B−57 (3)
C50—Ru3—P1—C3833.9 (3)P1—C32B—C37B—C36B165 (2)
Ru1—Ru3—P1—C38−63.6 (2)C32B—P1—C38—C39−84.6 (10)
C51—Ru3—P1—C32A−103.8 (6)C26A—P1—C38—C39175.9 (6)
C52—Ru3—P1—C32A−10.6 (6)C32A—P1—C38—C39−79.5 (6)
C50—Ru3—P1—C32A159.5 (6)C26B—P1—C38—C39166.2 (9)
Ru1—Ru3—P1—C32A62.1 (5)Ru3—P1—C38—C3948.8 (4)
C51—Ru3—P1—C26B15.3 (8)C32B—P1—C38—C43A41.5 (10)
C52—Ru3—P1—C26B108.5 (8)C26A—P1—C38—C43A−58.0 (7)
C50—Ru3—P1—C26B−81.4 (8)C32A—P1—C38—C43A46.6 (7)
Ru1—Ru3—P1—C26B−178.8 (8)C26B—P1—C38—C43A−67.7 (10)
C7—As1—C1—C2−100.0 (4)Ru3—P1—C38—C43A174.9 (4)
C13—As1—C1—C20.8 (5)C32B—P1—C38—C43B141.7 (11)
Ru1—As1—C1—C2129.2 (4)C26A—P1—C38—C43B42.3 (8)
C7—As1—C1—C680.1 (4)C32A—P1—C38—C43B146.8 (8)
C13—As1—C1—C6−179.1 (3)C26B—P1—C38—C43B32.6 (11)
Ru1—As1—C1—C6−50.7 (4)Ru3—P1—C38—C43B−84.8 (7)
C6—C1—C2—C30.6 (8)C43A—C38—C39—C4051.8 (7)
As1—C1—C2—C3−179.3 (5)C43B—C38—C39—C40−37.9 (8)
C1—C2—C3—C4−0.1 (10)P1—C38—C39—C40−177.4 (4)
C2—C3—C4—C5−0.8 (10)C38—C39—C40—C41B31.7 (13)
C3—C4—C5—C61.1 (8)C38—C39—C40—C41A−42.8 (9)
C2—C1—C6—C5−0.3 (7)C41B—C40—C41A—C42A−83.1 (10)
As1—C1—C6—C5179.6 (4)C39—C40—C41A—C42A38.5 (12)
C4—C5—C6—C1−0.5 (7)C40—C41A—C42A—C43A−46.1 (12)
C1—As1—C7—C850.2 (4)C41A—C42A—C43A—C3861.2 (10)
C13—As1—C7—C8−58.3 (4)C39—C38—C43A—C42A−63.0 (8)
Ru1—As1—C7—C8−179.6 (3)C43B—C38—C43A—C42A44.0 (8)
C1—As1—C7—C12−132.6 (4)P1—C38—C43A—C42A166.3 (6)
C13—As1—C7—C12118.9 (4)C41A—C40—C41B—C42B76.7 (11)
Ru1—As1—C7—C12−2.4 (4)C39—C40—C41B—C42B−30.4 (18)
C12—C7—C8—C90.3 (7)C40—C41B—C42B—C43B40.9 (17)
As1—C7—C8—C9177.5 (3)C41B—C42B—C43B—C38−54.4 (15)
C7—C8—C9—C10−0.1 (7)C39—C38—C43B—C42B52.8 (12)
C8—C9—C10—C11−0.2 (7)C43A—C38—C43B—C42B−52.9 (11)
C9—C10—C11—C120.2 (7)P1—C38—C43B—C42B−170.3 (8)
C8—C7—C12—C11−0.3 (7)

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
C31A—H31B···O80.972.563.481 (17)159
C32A—H32A···O90.982.473.157 (14)127
C43A—H43B···O9i0.972.182.954 (10)135
C5—H5A···Cg1ii0.932.943.728 (5)144
C10—H10A···Cg2iii0.932.903.651 (5)139
C16—H16A···Cg2iv0.932.963.718 (5)140
C22—H22A···Cg1v0.932.823.608 (5)143
C41B—H41D···Cg3ii0.972.623.420 (14)140

Symmetry codes: (i) x+1/2, −y+1/2, −z; (ii) x−1/2, y, −z−1/2; (iii) x+3/2, −y−1/2, −z; (iv) x−3/2, y, −z−1/2; (v) x+1, −y−1/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SJ2677).

References

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