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Acta Crystallogr Sect E Struct Rep Online. 2010 September 1; 66(Pt 9): m1152–m1153.
Published online 2010 August 21. doi:  10.1107/S1600536810032812
PMCID: PMC3007838

Bis([μ-bis­(diphenyl­arsino)methane-1:2κ2 As:As’]nona­carbonyl-1κ3 C,2κ3 C,3κ3 C-{tris­[4-(methyl­sulfan­yl)phen­yl]arsine-3κAs}-triangulo-triruthenium(0)) dichloro­methane monosolvate

Abstract

The asymmetric unit of the title triangulo-triruthenium compound, 2[Ru3(C25H22As2)(C21H21AsS3)(CO)9]·CH2Cl2, consists of one triangulo-triruthenium complex mol­ecule and one half of a dichloro­methane mol­ecule which lies across a crystallographic inversion center, leading to the disorder of this mol­ecule over two positions of equal occupancy. The bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate arsine ligand bonds to the third Ru atom. All arsine ligands are equatorial with respect to the Ru3 triangle. Each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three methyl­sulfanyl-substituted benzene rings make dihedral angles of 70.02 (8), 82.85 (9) and 89.49 (8)° with each other. The dihedral angles between the two phenyl rings are 78.25 (9) and 86.59 (9)° for the two diphenyl­arsino groups. In the crystal, weak inter­molecular C—H(...)π inter­actions are observed.

Related literature

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985 [triangle]); Bruce, Liddell, Hughes et al. (1988 [triangle]); Bruce, Liddell, Shawkataly et al. (1988 [triangle]). For related structures, see: Shawkataly et al. (1998 [triangle], 2004 [triangle]); Shawkataly, Khan, Sirat et al. (2010a [triangle],b [triangle]); Shawkataly, Khan, Yeap & Fun (2010a [triangle],b [triangle]). For the synthesis of bis­(diphenyl­arsino)methane, see: Bruce et al. (1983 [triangle]). For the stability of the temperature controller used in the data collection, see: Cosier & Glazer (1986 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-m1152-scheme1.jpg

Experimental

Crystal data

  • 2[Ru3(C25H22As2)(C21H21AsS3)(CO)9]·CH2Cl2
  • M r = 3029.01
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1152-efi1.jpg
  • a = 10.8807 (1) Å
  • b = 12.7494 (2) Å
  • c = 20.9320 (3) Å
  • α = 94.512 (1)°
  • β = 98.721 (1)°
  • γ = 102.855 (1)°
  • V = 2779.13 (6) Å3
  • Z = 1
  • Mo Kα radiation
  • μ = 2.79 mm−1
  • T = 100 K
  • 0.56 × 0.29 × 0.20 mm

Data collection

  • Bruker SMART APEXII CCD area-detector diffractometer
  • Absorption correction: multi-scan (SADABS; Bruker, 2009 [triangle]) T min = 0.306, T max = 0.605
  • 117127 measured reflections
  • 20038 independent reflections
  • 17668 reflections with I > 2σ(I)
  • R int = 0.027

Refinement

  • R[F 2 > 2σ(F 2)] = 0.023
  • wR(F 2) = 0.059
  • S = 1.01
  • 20038 reflections
  • 679 parameters
  • H-atom parameters constrained
  • Δρmax = 1.53 e Å−3
  • Δρmin = −1.28 e Å−3

Data collection: APEX2 (Bruker, 2009 [triangle]); cell refinement: SAINT (Bruker, 2009 [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/S1600536810032812/is2586sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810032812/is2586Isup2.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. SSS thanks USM for the Research Officer position. IAK is grateful to USM for a Visiting Researcher position. HKF and CSY thank USM for the Research University Golden Goose Grant 1001/PFIZIK/811012. CSY also thanks USM for the award of a USM Fellowship.

supplementary crystallographic information

Comment

Triangulo-triruthenium 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; Bruce, Liddell, Hughes et al., 1988; Bruce, Liddell, Shawkataly et al., 1988). 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; Shawkataly, Khan, Sirat et al., 2010a, b; Shawkataly, Khan, Yeap & Fun, 2010a, b). Herein we report the synthesis and structure of the title compound.

The asymmetry unit consists of one molecule of triangulo-triruthenium complex and half a molecule of dichloromethane solvent (Fig. 1). The dichloromethane solvent lies across a crystallographic inversion center leading to disorder of this solvent molecule over two positions. The geometric parameters of title compound are comparable to those found in related structures (Shawkataly, Khan, Sirat et al., 2010a,b; Shawkataly, Khan, Yeap & Fun, 2010a, b). The bis(diphenylarsino)methane ligand bridges the Ru1—Ru2 bond and the monodentate arsine ligand bonds to the Ru3 atom. All arsine ligands are equatorial with respect to the Ru3 triangle. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three arsine-substituted benzene rings make dihedral angles (C26–C31/C32–C37, C26–C31/C38–C43 and C32–C37/C38–C43) of 70.02 (8), 82.85 (9) and 89.49 (8)° with each other respectively. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 78.25 (9) and 86.59 (9)° for the two diphenylarsino groups respectively. The methylsulfanyl groups are nearly coplanar with the attached benzene rings [torsion angles C44–S1–C29–C30 = 10.75 (19), C45–S2–C35–C34 = -12.60 (18) and C46–S3–C41–C40 = 8.04 (18)°].

In the crystal packing, the molecules are stacked along a axis (Fig. 2). Weak intermolecular C—H···π interactions further stabilize the crystal structure (Table 1).

Experimental

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. Tris(4-(methylsulfanyl)phenyl)arsine was prepared from arsenic trichloride and 4-(methylsulfanyl)phenylmagnesium bromide in tetrahydrofuran and bis(diphenylarsino)methane (Bruce et al., 1983) was prepared by reported procedure. The title compound was obtained by refluxing equimolar quantities of Ru3(CO)10(µ-Ph2AsCH2AsPh2) and tris(4-(methylsulfanyl)phenyl)arsine in hexane under nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of CH3OH into CH2Cl2.

Refinement

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 groups. The highest peak and deepest hole in the difference Fourier map are located 0.74 and 0.65 Å, respectively, from atoms Ru1 and Cl1.

Figures

Fig. 1.
The molecular structure of the title compound with 50% probability ellipsoids for non-H atoms. Atoms with suffix A are generated by the symmetry operation (1 - x, 1 - y, -z).
Fig. 2.
The crystal packing of the title compound, viewed down the a axis, showing the molecules stacking along the a axis. The solvent molecule have been omitted for clarity.

Crystal data

2[Ru3(C25H22As2)(C21H21AsS3)(CO)9]·CH2Cl2Z = 1
Mr = 3029.01F(000) = 1490
Triclinic, P1Dx = 1.810 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.8807 (1) ÅCell parameters from 9631 reflections
b = 12.7494 (2) Åθ = 2.4–35.2°
c = 20.9320 (3) ŵ = 2.79 mm1
α = 94.512 (1)°T = 100 K
β = 98.721 (1)°Block, purple
γ = 102.855 (1)°0.56 × 0.29 × 0.20 mm
V = 2779.13 (6) Å3

Data collection

Bruker SMART APEXII CCD area-detector diffractometer20038 independent reflections
Radiation source: fine-focus sealed tube17668 reflections with I > 2σ(I)
graphiteRint = 0.027
[var phi] and ω scansθmax = 32.5°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2009)h = −16→15
Tmin = 0.306, Tmax = 0.605k = −19→19
117127 measured reflectionsl = −31→31

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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.059H-atom parameters constrained
S = 1.01w = 1/[σ2(Fo2) + (0.0279P)2 + 2.4001P] where P = (Fo2 + 2Fc2)/3
20038 reflections(Δ/σ)max = 0.002
679 parametersΔρmax = 1.53 e Å3
0 restraintsΔρmin = −1.28 e Å3

Special details

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.

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

xyzUiso*/UeqOcc. (<1)
Ru10.272408 (11)0.645285 (10)0.230778 (6)0.01503 (3)
Ru20.216711 (11)0.432162 (10)0.272952 (6)0.01492 (3)
Ru30.050554 (11)0.491262 (10)0.169550 (6)0.01399 (3)
As1−0.111284 (14)0.325798 (13)0.168266 (7)0.01466 (3)
As20.125920 (15)0.239793 (13)0.239305 (8)0.01539 (3)
As30.488230 (15)0.752248 (13)0.279266 (8)0.01564 (3)
S10.85951 (5)0.58930 (4)0.50245 (2)0.02778 (9)
S20.82705 (5)0.94466 (4)0.06532 (2)0.02522 (8)
S30.46708 (5)1.18489 (4)0.45993 (2)0.02596 (9)
O10.37182 (14)0.59457 (11)0.10436 (7)0.0281 (3)
O20.18120 (13)0.69186 (12)0.35930 (7)0.0282 (3)
O30.14505 (14)0.81485 (11)0.17632 (7)0.0293 (3)
O40.38610 (13)0.40882 (12)0.39778 (7)0.0297 (3)
O50.43725 (13)0.43147 (12)0.19702 (7)0.0293 (3)
O60.01003 (12)0.46497 (11)0.35320 (6)0.0241 (2)
O70.19057 (13)0.36294 (11)0.08694 (6)0.0256 (3)
O8−0.05033 (15)0.58824 (13)0.05006 (7)0.0326 (3)
O9−0.07202 (13)0.63293 (11)0.25395 (7)0.0277 (3)
C1−0.20996 (14)0.31631 (13)0.23781 (7)0.0176 (3)
C2−0.27612 (16)0.39622 (15)0.24823 (8)0.0211 (3)
H2A−0.27970.44750.21920.025*
C3−0.33693 (17)0.39948 (17)0.30216 (9)0.0262 (3)
H3A−0.38070.45300.30910.031*
C4−0.33218 (18)0.32294 (18)0.34550 (9)0.0298 (4)
H4A−0.37160.32580.38180.036*
C5−0.26847 (19)0.24217 (18)0.33449 (9)0.0300 (4)
H5A−0.26690.19000.36300.036*
C6−0.20672 (16)0.23860 (15)0.28098 (8)0.0225 (3)
H6A−0.16350.18460.27410.027*
C7−0.23627 (15)0.27070 (13)0.08947 (8)0.0180 (3)
C8−0.36537 (17)0.23264 (17)0.08984 (9)0.0264 (4)
H8A−0.39640.23470.12880.032*
C9−0.44931 (19)0.19095 (19)0.03128 (10)0.0336 (4)
H9A−0.53630.16540.03140.040*
C10−0.4035 (2)0.18778 (17)−0.02634 (9)0.0315 (4)
H10A−0.45950.1598−0.06510.038*
C11−0.2739 (2)0.22627 (17)−0.02666 (9)0.0286 (4)
H11A−0.24310.2239−0.06570.034*
C12−0.19026 (17)0.26813 (15)0.03093 (8)0.0232 (3)
H12A−0.10350.29450.03050.028*
C13−0.03139 (15)0.20321 (13)0.17414 (8)0.0188 (3)
H13A−0.01150.18230.13200.023*
H13B−0.09100.14200.18570.023*
C140.08324 (15)0.14022 (14)0.30329 (8)0.0206 (3)
C150.10313 (19)0.17852 (16)0.36886 (9)0.0261 (3)
H15A0.13160.25240.38220.031*
C160.0804 (2)0.10586 (19)0.41471 (11)0.0369 (5)
H16A0.09420.13130.45870.044*
C170.0370 (2)−0.00437 (19)0.39450 (12)0.0414 (5)
H17A0.0211−0.05260.42500.050*
C180.0172 (2)−0.04314 (18)0.32887 (12)0.0386 (5)
H18A−0.0116−0.11710.31560.046*
C190.04048 (19)0.02893 (15)0.28324 (10)0.0282 (4)
H19A0.02770.00320.23930.034*
C200.23331 (15)0.16287 (13)0.19779 (8)0.0187 (3)
C210.18807 (17)0.09077 (15)0.14123 (9)0.0228 (3)
H21A0.10320.07900.12090.027*
C220.27003 (18)0.03630 (15)0.11511 (9)0.0256 (3)
H22A0.2403−0.01110.07700.031*
C230.39557 (18)0.05293 (15)0.14596 (10)0.0267 (4)
H23A0.45020.01650.12850.032*
C240.44057 (17)0.12360 (15)0.20272 (10)0.0266 (4)
H24A0.52490.13380.22350.032*
C250.35995 (16)0.17917 (14)0.22860 (9)0.0222 (3)
H25A0.39040.22720.26640.027*
C260.60497 (15)0.69454 (13)0.33824 (8)0.0179 (3)
C270.55549 (16)0.63871 (14)0.38685 (8)0.0197 (3)
H27A0.46760.62180.38610.024*
C280.63538 (17)0.60794 (15)0.43627 (8)0.0219 (3)
H28A0.60100.57170.46870.026*
C290.76761 (17)0.63140 (14)0.43739 (8)0.0213 (3)
C300.81776 (17)0.68450 (16)0.38786 (9)0.0238 (3)
H30A0.90530.69870.38750.029*
C310.73621 (16)0.71633 (15)0.33882 (8)0.0222 (3)
H31A0.77010.75250.30620.027*
C320.59651 (15)0.80848 (13)0.21796 (8)0.0178 (3)
C330.64666 (17)0.73863 (14)0.17964 (9)0.0218 (3)
H33A0.63040.66530.18480.026*
C340.72016 (17)0.77792 (14)0.13421 (9)0.0223 (3)
H34A0.75470.73120.10990.027*
C350.74257 (15)0.88703 (14)0.12467 (8)0.0190 (3)
C360.69174 (15)0.95644 (13)0.16237 (8)0.0198 (3)
H36A0.70531.02920.15600.024*
C370.62117 (15)0.91777 (13)0.20920 (8)0.0188 (3)
H37A0.59020.96530.23490.023*
C380.48767 (16)0.88287 (13)0.33407 (8)0.0184 (3)
C390.58630 (17)0.92682 (14)0.38610 (9)0.0227 (3)
H39A0.65510.89480.39420.027*
C400.58315 (18)1.01828 (15)0.42624 (9)0.0241 (3)
H40A0.64911.04640.46120.029*
C410.48100 (17)1.06787 (14)0.41394 (8)0.0209 (3)
C420.38201 (18)1.02368 (15)0.36202 (9)0.0243 (3)
H42A0.31341.05590.35370.029*
C430.38508 (17)0.93201 (15)0.32264 (9)0.0231 (3)
H43A0.31810.90290.28820.028*
C441.02155 (19)0.65328 (19)0.49658 (10)0.0325 (4)
H44A1.07890.63790.53220.049*
H44B1.03100.73020.49810.049*
H44C1.04120.62590.45620.049*
C450.9014 (2)0.84077 (18)0.03799 (11)0.0369 (5)
H45A0.96140.86960.01090.055*
H45B0.83700.78130.01350.055*
H45C0.94540.81600.07490.055*
C460.6196 (2)1.22632 (18)0.51238 (10)0.0333 (4)
H46A0.62841.29700.53470.050*
H46B0.68641.22840.48700.050*
H46C0.62581.17570.54360.050*
C470.33234 (16)0.60875 (13)0.15090 (8)0.0202 (3)
C480.21287 (16)0.66581 (14)0.31181 (8)0.0211 (3)
C490.20010 (16)0.75351 (14)0.19592 (8)0.0211 (3)
C500.32480 (16)0.41959 (14)0.35019 (8)0.0211 (3)
C510.35334 (16)0.43797 (14)0.22309 (8)0.0210 (3)
C520.08354 (16)0.45379 (13)0.32111 (8)0.0194 (3)
C530.14356 (15)0.41231 (14)0.11959 (8)0.0193 (3)
C54−0.01435 (16)0.55206 (14)0.09543 (8)0.0204 (3)
C55−0.02389 (15)0.57839 (14)0.22517 (8)0.0194 (3)
Cl10.61496 (8)0.49986 (6)0.04724 (4)0.05599 (17)
C560.4702 (4)0.4354 (3)0.0093 (2)0.0350 (9)0.50
H56A0.41920.41530.04200.042*0.50
H56B0.47880.3697−0.01330.042*0.50

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ru10.01532 (5)0.01408 (5)0.01565 (5)0.00296 (4)0.00280 (4)0.00285 (4)
Ru20.01539 (5)0.01395 (5)0.01464 (5)0.00296 (4)0.00039 (4)0.00277 (4)
Ru30.01374 (5)0.01517 (5)0.01342 (5)0.00404 (4)0.00224 (4)0.00237 (4)
As10.01356 (6)0.01611 (7)0.01415 (7)0.00352 (5)0.00181 (5)0.00206 (5)
As20.01483 (6)0.01406 (7)0.01690 (7)0.00340 (5)0.00131 (5)0.00233 (5)
As30.01571 (7)0.01459 (7)0.01686 (7)0.00385 (5)0.00312 (5)0.00201 (5)
S10.0283 (2)0.0360 (2)0.02015 (19)0.01163 (18)−0.00015 (16)0.00650 (17)
S20.0289 (2)0.0235 (2)0.0238 (2)0.00305 (16)0.01031 (16)0.00445 (16)
S30.0324 (2)0.0214 (2)0.0243 (2)0.00701 (17)0.00700 (16)−0.00196 (16)
O10.0348 (7)0.0263 (7)0.0255 (6)0.0071 (5)0.0118 (5)0.0039 (5)
O20.0297 (7)0.0293 (7)0.0230 (6)0.0003 (5)0.0085 (5)−0.0021 (5)
O30.0330 (7)0.0267 (7)0.0306 (7)0.0124 (6)0.0025 (5)0.0078 (5)
O40.0287 (7)0.0329 (7)0.0247 (6)0.0043 (5)−0.0036 (5)0.0104 (5)
O50.0242 (6)0.0355 (7)0.0346 (7)0.0131 (5)0.0104 (5)0.0148 (6)
O60.0237 (6)0.0285 (6)0.0201 (6)0.0054 (5)0.0044 (4)0.0034 (5)
O70.0255 (6)0.0286 (7)0.0234 (6)0.0089 (5)0.0051 (5)−0.0027 (5)
O80.0372 (8)0.0368 (8)0.0266 (7)0.0141 (6)0.0015 (6)0.0129 (6)
O90.0254 (6)0.0293 (7)0.0303 (7)0.0098 (5)0.0081 (5)−0.0019 (5)
C10.0148 (6)0.0216 (7)0.0156 (6)0.0025 (5)0.0023 (5)0.0025 (5)
C20.0186 (7)0.0252 (8)0.0200 (7)0.0055 (6)0.0045 (5)0.0033 (6)
C30.0202 (7)0.0358 (10)0.0229 (8)0.0077 (7)0.0057 (6)−0.0012 (7)
C40.0231 (8)0.0457 (12)0.0202 (8)0.0035 (8)0.0078 (6)0.0061 (8)
C50.0275 (9)0.0385 (11)0.0250 (8)0.0045 (8)0.0073 (7)0.0138 (8)
C60.0198 (7)0.0252 (8)0.0226 (8)0.0041 (6)0.0040 (6)0.0074 (6)
C70.0182 (6)0.0186 (7)0.0163 (6)0.0040 (5)0.0005 (5)0.0026 (5)
C80.0201 (7)0.0362 (10)0.0197 (7)0.0008 (7)0.0008 (6)0.0052 (7)
C90.0226 (8)0.0427 (12)0.0280 (9)−0.0029 (8)−0.0038 (7)0.0055 (8)
C100.0329 (9)0.0332 (10)0.0225 (8)0.0050 (8)−0.0076 (7)−0.0007 (7)
C110.0357 (10)0.0338 (10)0.0166 (7)0.0121 (8)0.0011 (7)0.0004 (7)
C120.0242 (8)0.0278 (9)0.0183 (7)0.0082 (6)0.0033 (6)0.0021 (6)
C130.0164 (6)0.0172 (7)0.0218 (7)0.0047 (5)0.0001 (5)0.0006 (6)
C140.0179 (7)0.0202 (7)0.0244 (8)0.0043 (6)0.0037 (6)0.0076 (6)
C150.0319 (9)0.0251 (9)0.0238 (8)0.0081 (7)0.0090 (7)0.0069 (7)
C160.0492 (12)0.0389 (11)0.0288 (10)0.0136 (10)0.0163 (9)0.0146 (9)
C170.0501 (13)0.0350 (11)0.0430 (12)0.0064 (10)0.0160 (10)0.0228 (10)
C180.0409 (11)0.0230 (9)0.0498 (13)−0.0013 (8)0.0095 (10)0.0140 (9)
C190.0298 (9)0.0205 (8)0.0314 (9)0.0004 (7)0.0037 (7)0.0059 (7)
C200.0177 (6)0.0167 (7)0.0225 (7)0.0051 (5)0.0037 (5)0.0041 (6)
C210.0222 (7)0.0226 (8)0.0239 (8)0.0083 (6)0.0018 (6)0.0002 (6)
C220.0297 (9)0.0242 (8)0.0253 (8)0.0118 (7)0.0049 (7)0.0009 (7)
C230.0255 (8)0.0244 (8)0.0345 (9)0.0111 (7)0.0100 (7)0.0046 (7)
C240.0180 (7)0.0256 (9)0.0374 (10)0.0081 (6)0.0039 (7)0.0048 (7)
C250.0182 (7)0.0201 (8)0.0272 (8)0.0050 (6)0.0006 (6)0.0016 (6)
C260.0189 (7)0.0181 (7)0.0169 (7)0.0054 (5)0.0023 (5)0.0016 (5)
C270.0194 (7)0.0194 (7)0.0201 (7)0.0042 (6)0.0036 (5)0.0018 (6)
C280.0228 (7)0.0240 (8)0.0189 (7)0.0050 (6)0.0036 (6)0.0040 (6)
C290.0244 (7)0.0219 (8)0.0176 (7)0.0079 (6)0.0012 (6)0.0010 (6)
C300.0199 (7)0.0309 (9)0.0227 (8)0.0097 (6)0.0036 (6)0.0058 (7)
C310.0198 (7)0.0266 (8)0.0224 (8)0.0077 (6)0.0052 (6)0.0076 (6)
C320.0172 (6)0.0179 (7)0.0182 (7)0.0037 (5)0.0028 (5)0.0027 (5)
C330.0260 (8)0.0162 (7)0.0241 (8)0.0045 (6)0.0079 (6)0.0029 (6)
C340.0253 (8)0.0197 (8)0.0227 (8)0.0057 (6)0.0077 (6)0.0001 (6)
C350.0179 (7)0.0198 (7)0.0174 (7)0.0015 (5)0.0022 (5)0.0017 (6)
C360.0189 (7)0.0163 (7)0.0237 (7)0.0030 (5)0.0031 (6)0.0036 (6)
C370.0185 (7)0.0169 (7)0.0207 (7)0.0041 (5)0.0035 (5)0.0011 (6)
C380.0203 (7)0.0164 (7)0.0188 (7)0.0046 (5)0.0043 (5)0.0019 (5)
C390.0222 (7)0.0207 (8)0.0242 (8)0.0056 (6)0.0009 (6)0.0014 (6)
C400.0271 (8)0.0209 (8)0.0223 (8)0.0057 (6)−0.0001 (6)−0.0004 (6)
C410.0272 (8)0.0170 (7)0.0198 (7)0.0054 (6)0.0082 (6)0.0025 (6)
C420.0252 (8)0.0237 (8)0.0252 (8)0.0096 (6)0.0041 (6)0.0005 (6)
C430.0235 (7)0.0230 (8)0.0229 (8)0.0080 (6)0.0014 (6)−0.0002 (6)
C440.0257 (9)0.0432 (12)0.0301 (9)0.0143 (8)0.0003 (7)0.0045 (8)
C450.0490 (13)0.0332 (11)0.0345 (11)0.0128 (9)0.0222 (9)0.0024 (8)
C460.0355 (10)0.0325 (10)0.0286 (9)0.0035 (8)0.0077 (8)−0.0062 (8)
C470.0223 (7)0.0161 (7)0.0217 (7)0.0036 (6)0.0031 (6)0.0037 (6)
C480.0190 (7)0.0209 (8)0.0213 (7)0.0009 (6)0.0023 (6)0.0032 (6)
C490.0231 (7)0.0204 (7)0.0194 (7)0.0036 (6)0.0045 (6)0.0031 (6)
C500.0203 (7)0.0198 (7)0.0221 (7)0.0027 (6)0.0018 (6)0.0044 (6)
C510.0198 (7)0.0211 (8)0.0219 (7)0.0051 (6)0.0007 (6)0.0076 (6)
C520.0207 (7)0.0183 (7)0.0167 (7)0.0025 (6)−0.0013 (5)0.0026 (5)
C530.0188 (7)0.0196 (7)0.0186 (7)0.0035 (6)0.0019 (5)0.0027 (6)
C540.0197 (7)0.0222 (8)0.0198 (7)0.0059 (6)0.0035 (5)0.0034 (6)
C550.0191 (7)0.0209 (7)0.0187 (7)0.0054 (6)0.0034 (5)0.0026 (6)
Cl10.0662 (4)0.0542 (4)0.0519 (4)0.0291 (3)0.0076 (3)−0.0050 (3)
C560.040 (2)0.0269 (19)0.042 (2)0.0097 (16)0.0186 (18)0.0030 (17)

Geometric parameters (Å, °)

Ru1—C491.8768 (17)C15—C161.397 (3)
Ru1—C481.9246 (17)C15—H15A0.9300
Ru1—C471.9445 (17)C16—C171.388 (3)
Ru1—As32.4574 (2)C16—H16A0.9300
Ru1—Ru32.80754 (17)C17—C181.391 (4)
Ru1—Ru22.88731 (18)C17—H17A0.9300
Ru2—C501.8897 (17)C18—C191.389 (3)
Ru2—C511.9335 (18)C18—H18A0.9300
Ru2—C521.9414 (17)C19—H19A0.9300
Ru2—As22.4344 (2)C20—C211.393 (2)
Ru2—Ru32.86304 (17)C20—C251.393 (2)
Ru3—C541.8993 (17)C21—C221.393 (2)
Ru3—C551.9309 (17)C21—H21A0.9300
Ru3—C531.9338 (17)C22—C231.382 (3)
Ru3—As12.4240 (2)C22—H22A0.9300
As1—C11.9314 (16)C23—C241.386 (3)
As1—C71.9431 (16)C23—H23A0.9300
As1—C131.9534 (16)C24—C251.388 (3)
As2—C201.9406 (16)C24—H24A0.9300
As2—C141.9532 (16)C25—H25A0.9300
As2—C131.9608 (16)C26—C311.391 (2)
As3—C261.9395 (16)C26—C271.393 (2)
As3—C321.9432 (16)C27—C281.387 (2)
As3—C381.9482 (16)C27—H27A0.9300
S1—C291.7560 (17)C28—C291.399 (2)
S1—C441.797 (2)C28—H28A0.9300
S2—C351.7657 (17)C29—C301.396 (2)
S2—C451.798 (2)C30—C311.398 (2)
S3—C411.7589 (17)C30—H30A0.9300
S3—C461.790 (2)C31—H31A0.9300
O1—C471.140 (2)C32—C371.391 (2)
O2—C481.149 (2)C32—C331.404 (2)
O3—C491.150 (2)C33—C341.387 (2)
O4—C501.148 (2)C33—H33A0.9300
O5—C511.147 (2)C34—C351.394 (2)
O6—C521.144 (2)C34—H34A0.9300
O7—C531.143 (2)C35—C361.397 (2)
O8—C541.142 (2)C36—C371.389 (2)
O9—C551.146 (2)C36—H36A0.9300
C1—C21.394 (2)C37—H37A0.9300
C1—C61.395 (2)C38—C391.391 (2)
C2—C31.395 (2)C38—C431.396 (2)
C2—H2A0.9300C39—C401.392 (3)
C3—C41.388 (3)C39—H39A0.9300
C3—H3A0.9300C40—C411.397 (2)
C4—C51.387 (3)C40—H40A0.9300
C4—H4A0.9300C41—C421.392 (3)
C5—C61.394 (3)C42—C431.386 (3)
C5—H5A0.9300C42—H42A0.9300
C6—H6A0.9300C43—H43A0.9300
C7—C81.382 (2)C44—H44A0.9600
C7—C121.393 (2)C44—H44B0.9600
C8—C91.400 (3)C44—H44C0.9600
C8—H8A0.9300C45—H45A0.9600
C9—C101.374 (3)C45—H45B0.9600
C9—H9A0.9300C45—H45C0.9600
C10—C111.388 (3)C46—H46A0.9600
C10—H10A0.9300C46—H46B0.9600
C11—C121.384 (2)C46—H46C0.9600
C11—H11A0.9300Cl1—C561.652 (5)
C12—H12A0.9300Cl1—C56i1.761 (5)
C13—H13A0.9700C56—Cl1i1.761 (5)
C13—H13B0.9700C56—H56A0.9599
C14—C151.388 (3)C56—H56B0.9599
C14—C191.400 (3)
C49—Ru1—C4892.55 (7)C16—C17—H17A119.8
C49—Ru1—C4792.99 (7)C18—C17—H17A119.8
C48—Ru1—C47173.85 (7)C19—C18—C17119.8 (2)
C49—Ru1—As3100.49 (5)C19—C18—H18A120.1
C48—Ru1—As391.09 (5)C17—C18—H18A120.1
C47—Ru1—As390.53 (5)C18—C19—C14120.0 (2)
C49—Ru1—Ru388.60 (5)C18—C19—H19A120.0
C48—Ru1—Ru395.13 (5)C14—C19—H19A120.0
C47—Ru1—Ru382.34 (5)C21—C20—C25119.90 (16)
As3—Ru1—Ru3168.757 (7)C21—C20—As2123.14 (12)
C49—Ru1—Ru2144.64 (5)C25—C20—As2116.92 (13)
C48—Ru1—Ru275.31 (5)C20—C21—C22119.93 (16)
C47—Ru1—Ru298.60 (5)C20—C21—H21A120.0
As3—Ru1—Ru2112.611 (6)C22—C21—H21A120.0
Ru3—Ru1—Ru260.344 (4)C23—C22—C21119.83 (18)
C50—Ru2—C5191.86 (7)C23—C22—H22A120.1
C50—Ru2—C5291.39 (7)C21—C22—H22A120.1
C51—Ru2—C52169.68 (7)C22—C23—C24120.43 (17)
C50—Ru2—As297.87 (5)C22—C23—H23A119.8
C51—Ru2—As293.44 (5)C24—C23—H23A119.8
C52—Ru2—As295.82 (5)C23—C24—C25120.09 (17)
C50—Ru2—Ru3168.52 (5)C23—C24—H24A120.0
C51—Ru2—Ru393.27 (5)C25—C24—H24A120.0
C52—Ru2—Ru381.86 (5)C24—C25—C20119.82 (17)
As2—Ru2—Ru392.069 (6)C24—C25—H25A120.1
C50—Ru2—Ru1113.64 (5)C20—C25—H25A120.1
C51—Ru2—Ru172.94 (5)C31—C26—C27118.87 (15)
C52—Ru2—Ru196.79 (5)C31—C26—As3123.38 (12)
As2—Ru2—Ru1145.613 (7)C27—C26—As3117.35 (12)
Ru3—Ru2—Ru158.448 (5)C28—C27—C26120.97 (15)
C54—Ru3—C5590.94 (7)C28—C27—H27A119.5
C54—Ru3—C5392.15 (7)C26—C27—H27A119.5
C55—Ru3—C53173.56 (7)C27—C28—C29120.10 (16)
C54—Ru3—As1103.19 (5)C27—C28—H28A120.0
C55—Ru3—As194.78 (5)C29—C28—H28A120.0
C53—Ru3—As190.01 (5)C30—C29—C28119.37 (15)
C54—Ru3—Ru1105.36 (5)C30—C29—S1124.46 (13)
C55—Ru3—Ru180.28 (5)C28—C29—S1116.17 (13)
C53—Ru3—Ru193.45 (5)C29—C30—C31119.87 (16)
As1—Ru3—Ru1151.077 (7)C29—C30—H30A120.1
C54—Ru3—Ru2163.58 (5)C31—C30—H30A120.1
C55—Ru3—Ru295.58 (5)C26—C31—C30120.78 (16)
C53—Ru3—Ru279.99 (5)C26—C31—H31A119.6
As1—Ru3—Ru291.288 (6)C30—C31—H31A119.6
Ru1—Ru3—Ru261.208 (4)C37—C32—C33118.79 (15)
C1—As1—C7104.88 (7)C37—C32—As3120.65 (12)
C1—As1—C13103.91 (7)C33—C32—As3120.51 (12)
C7—As1—C1398.75 (7)C34—C33—C32120.63 (16)
C1—As1—Ru3117.77 (5)C34—C33—H33A119.7
C7—As1—Ru3119.04 (5)C32—C33—H33A119.7
C13—As1—Ru3109.90 (5)C33—C34—C35120.42 (16)
C20—As2—C1497.80 (7)C33—C34—H34A119.8
C20—As2—C13101.07 (7)C35—C34—H34A119.8
C14—As2—C13102.17 (7)C34—C35—C36118.99 (15)
C20—As2—Ru2115.82 (5)C34—C35—S2124.43 (13)
C14—As2—Ru2120.82 (5)C36—C35—S2116.54 (13)
C13—As2—Ru2115.87 (5)C37—C36—C35120.63 (15)
C26—As3—C32101.35 (7)C37—C36—H36A119.7
C26—As3—C3899.20 (7)C35—C36—H36A119.7
C32—As3—C38102.56 (7)C36—C37—C32120.51 (15)
C26—As3—Ru1121.96 (5)C36—C37—H37A119.7
C32—As3—Ru1115.64 (5)C32—C37—H37A119.7
C38—As3—Ru1113.24 (5)C39—C38—C43118.88 (16)
C29—S1—C44103.72 (9)C39—C38—As3121.12 (12)
C35—S2—C45103.76 (9)C43—C38—As3119.97 (13)
C41—S3—C46102.37 (9)C38—C39—C40120.73 (16)
C2—C1—C6119.66 (15)C38—C39—H39A119.6
C2—C1—As1118.17 (12)C40—C39—H39A119.6
C6—C1—As1121.88 (13)C39—C40—C41120.05 (16)
C1—C2—C3120.11 (16)C39—C40—H40A120.0
C1—C2—H2A119.9C41—C40—H40A120.0
C3—C2—H2A119.9C42—C41—C40119.24 (16)
C4—C3—C2120.12 (18)C42—C41—S3116.25 (13)
C4—C3—H3A119.9C40—C41—S3124.51 (14)
C2—C3—H3A119.9C43—C42—C41120.43 (16)
C5—C4—C3119.80 (17)C43—C42—H42A119.8
C5—C4—H4A120.1C41—C42—H42A119.8
C3—C4—H4A120.1C42—C43—C38120.67 (16)
C4—C5—C6120.52 (17)C42—C43—H43A119.7
C4—C5—H5A119.7C38—C43—H43A119.7
C6—C5—H5A119.7S1—C44—H44A109.5
C5—C6—C1119.76 (17)S1—C44—H44B109.5
C5—C6—H6A120.1H44A—C44—H44B109.5
C1—C6—H6A120.1S1—C44—H44C109.5
C8—C7—C12119.96 (15)H44A—C44—H44C109.5
C8—C7—As1122.94 (12)H44B—C44—H44C109.5
C12—C7—As1117.08 (12)S2—C45—H45A109.5
C7—C8—C9119.75 (17)S2—C45—H45B109.5
C7—C8—H8A120.1H45A—C45—H45B109.5
C9—C8—H8A120.1S2—C45—H45C109.5
C10—C9—C8120.16 (18)H45A—C45—H45C109.5
C10—C9—H9A119.9H45B—C45—H45C109.5
C8—C9—H9A119.9S3—C46—H46A109.5
C9—C10—C11120.02 (17)S3—C46—H46B109.5
C9—C10—H10A120.0H46A—C46—H46B109.5
C11—C10—H10A120.0S3—C46—H46C109.5
C12—C11—C10120.23 (18)H46A—C46—H46C109.5
C12—C11—H11A119.9H46B—C46—H46C109.5
C10—C11—H11A119.9O1—C47—Ru1175.32 (15)
C11—C12—C7119.86 (17)O2—C48—Ru1171.28 (15)
C11—C12—H12A120.1O3—C49—Ru1173.42 (16)
C7—C12—H12A120.1O4—C50—Ru2177.06 (16)
As1—C13—As2111.17 (8)O5—C51—Ru2172.10 (15)
As1—C13—H13A109.4O6—C52—Ru2175.31 (14)
As2—C13—H13A109.4O7—C53—Ru3175.10 (15)
As1—C13—H13B109.4O8—C54—Ru3177.98 (16)
As2—C13—H13B109.4O9—C55—Ru3174.75 (15)
H13A—C13—H13B108.0C56—Cl1—C56i60.8 (3)
C15—C14—C19119.98 (16)Cl1—C56—C56i62.8 (3)
C15—C14—As2120.30 (13)Cl1—C56—Cl1i119.2 (2)
C19—C14—As2119.58 (14)C56i—C56—Cl1i56.5 (3)
C14—C15—C16119.89 (19)Cl1—C56—H56A107.5
C14—C15—H15A120.1C56i—C56—H56A127.4
C16—C15—H15A120.1Cl1i—C56—H56A108.3
C17—C16—C15119.9 (2)Cl1—C56—H56B106.7
C17—C16—H16A120.1C56i—C56—H56B125.3
C15—C16—H16A120.1Cl1i—C56—H56B107.3
C16—C17—C18120.42 (19)H56A—C56—H56B107.3
C49—Ru1—Ru2—C50−138.92 (11)C7—As1—C1—C2−79.09 (14)
C48—Ru1—Ru2—C50−65.79 (8)C13—As1—C1—C2177.73 (13)
C47—Ru1—Ru2—C50113.36 (8)Ru3—As1—C1—C255.95 (14)
As3—Ru1—Ru2—C5019.17 (6)C7—As1—C1—C6107.05 (14)
Ru3—Ru1—Ru2—C50−170.60 (6)C13—As1—C1—C63.88 (15)
C49—Ru1—Ru2—C51136.67 (10)Ru3—As1—C1—C6−117.91 (13)
C48—Ru1—Ru2—C51−150.20 (7)C6—C1—C2—C31.1 (2)
C47—Ru1—Ru2—C5128.95 (7)As1—C1—C2—C3−172.93 (13)
As3—Ru1—Ru2—C51−65.25 (5)C1—C2—C3—C4−0.2 (3)
Ru3—Ru1—Ru2—C51104.98 (5)C2—C3—C4—C5−1.0 (3)
C49—Ru1—Ru2—C52−44.40 (10)C3—C4—C5—C61.4 (3)
C48—Ru1—Ru2—C5228.73 (7)C4—C5—C6—C1−0.6 (3)
C47—Ru1—Ru2—C52−152.12 (7)C2—C1—C6—C5−0.7 (3)
As3—Ru1—Ru2—C52113.69 (5)As1—C1—C6—C5173.10 (14)
Ru3—Ru1—Ru2—C52−76.08 (5)C1—As1—C7—C8−1.40 (17)
C49—Ru1—Ru2—As266.38 (9)C13—As1—C7—C8105.61 (16)
C48—Ru1—Ru2—As2139.51 (5)Ru3—As1—C7—C8−135.74 (14)
C47—Ru1—Ru2—As2−41.34 (5)C1—As1—C7—C12−179.85 (13)
As3—Ru1—Ru2—As2−135.534 (11)C13—As1—C7—C12−72.84 (14)
Ru3—Ru1—Ru2—As234.694 (11)Ru3—As1—C7—C1245.81 (15)
C49—Ru1—Ru2—Ru331.68 (9)C12—C7—C8—C90.4 (3)
C48—Ru1—Ru2—Ru3104.81 (5)As1—C7—C8—C9−177.99 (16)
C47—Ru1—Ru2—Ru3−76.04 (5)C7—C8—C9—C100.1 (3)
As3—Ru1—Ru2—Ru3−170.228 (7)C8—C9—C10—C11−0.2 (3)
C49—Ru1—Ru3—C5427.93 (7)C9—C10—C11—C12−0.1 (3)
C48—Ru1—Ru3—C54120.36 (7)C10—C11—C12—C70.6 (3)
C47—Ru1—Ru3—C54−65.28 (7)C8—C7—C12—C11−0.7 (3)
As3—Ru1—Ru3—C54−116.29 (6)As1—C7—C12—C11177.76 (14)
Ru2—Ru1—Ru3—C54−169.77 (5)C1—As1—C13—As2−83.61 (9)
C49—Ru1—Ru3—C55−60.37 (7)C7—As1—C13—As2168.59 (8)
C48—Ru1—Ru3—C5532.06 (7)Ru3—As1—C13—As243.27 (9)
C47—Ru1—Ru3—C55−153.57 (7)C20—As2—C13—As1−142.99 (8)
As3—Ru1—Ru3—C55155.41 (6)C14—As2—C13—As1116.42 (9)
Ru2—Ru1—Ru3—C55101.93 (5)Ru2—As2—C13—As1−16.97 (10)
C49—Ru1—Ru3—C53121.11 (7)C20—As2—C14—C15127.08 (15)
C48—Ru1—Ru3—C53−146.46 (7)C13—As2—C14—C15−129.76 (15)
C47—Ru1—Ru3—C5327.90 (7)Ru2—As2—C14—C150.66 (16)
As3—Ru1—Ru3—C53−23.11 (6)C20—As2—C14—C19−48.66 (15)
Ru2—Ru1—Ru3—C53−76.59 (5)C13—As2—C14—C1954.50 (15)
C49—Ru1—Ru3—As1−142.62 (5)Ru2—As2—C14—C19−175.08 (12)
C48—Ru1—Ru3—As1−50.18 (5)C19—C14—C15—C160.0 (3)
C47—Ru1—Ru3—As1124.18 (5)As2—C14—C15—C16−175.76 (16)
As3—Ru1—Ru3—As173.16 (4)C14—C15—C16—C17−0.5 (3)
Ru2—Ru1—Ru3—As119.685 (13)C15—C16—C17—C180.6 (4)
C49—Ru1—Ru3—Ru2−162.30 (5)C16—C17—C18—C19−0.2 (4)
C48—Ru1—Ru3—Ru2−69.87 (5)C17—C18—C19—C14−0.3 (3)
C47—Ru1—Ru3—Ru2104.50 (5)C15—C14—C19—C180.4 (3)
As3—Ru1—Ru3—Ru253.48 (3)As2—C14—C19—C18176.16 (16)
C50—Ru2—Ru3—C5486.0 (3)C14—As2—C20—C2195.77 (15)
C51—Ru2—Ru3—C54−30.4 (2)C13—As2—C20—C21−8.33 (16)
C52—Ru2—Ru3—C54140.46 (19)Ru2—As2—C20—C21−134.38 (13)
As2—Ru2—Ru3—C54−123.96 (19)C14—As2—C20—C25−81.72 (14)
Ru1—Ru2—Ru3—C5437.28 (19)C13—As2—C20—C25174.18 (13)
C50—Ru2—Ru3—C55−27.0 (3)Ru2—As2—C20—C2548.13 (14)
C51—Ru2—Ru3—C55−143.36 (7)C25—C20—C21—C22−0.9 (3)
C52—Ru2—Ru3—C5527.50 (7)As2—C20—C21—C22−178.32 (14)
As2—Ru2—Ru3—C55123.08 (5)C20—C21—C22—C230.9 (3)
Ru1—Ru2—Ru3—C55−75.69 (5)C21—C22—C23—C24−0.1 (3)
C50—Ru2—Ru3—C53148.3 (3)C22—C23—C24—C25−0.7 (3)
C51—Ru2—Ru3—C5331.93 (7)C23—C24—C25—C200.7 (3)
C52—Ru2—Ru3—C53−157.22 (7)C21—C20—C25—C240.1 (3)
As2—Ru2—Ru3—C53−61.64 (5)As2—C20—C25—C24177.69 (14)
Ru1—Ru2—Ru3—C5399.60 (5)C32—As3—C26—C3112.40 (16)
C50—Ru2—Ru3—As1−121.9 (3)C38—As3—C26—C31−92.50 (15)
C51—Ru2—Ru3—As1121.71 (5)Ru1—As3—C26—C31142.60 (13)
C52—Ru2—Ru3—As1−67.44 (5)C32—As3—C26—C27−174.97 (13)
As2—Ru2—Ru3—As128.143 (7)C38—As3—C26—C2780.12 (14)
Ru1—Ru2—Ru3—As1−170.622 (7)Ru1—As3—C26—C27−44.78 (15)
C50—Ru2—Ru3—Ru148.7 (3)C31—C26—C27—C281.9 (3)
C51—Ru2—Ru3—Ru1−67.67 (5)As3—C26—C27—C28−171.04 (13)
C52—Ru2—Ru3—Ru1103.18 (5)C26—C27—C28—C29−0.9 (3)
As2—Ru2—Ru3—Ru1−161.235 (7)C27—C28—C29—C30−0.9 (3)
C54—Ru3—As1—C1−113.07 (7)C27—C28—C29—S1179.66 (14)
C55—Ru3—As1—C1−20.97 (7)C44—S1—C29—C3010.75 (19)
C53—Ru3—As1—C1154.72 (7)C44—S1—C29—C28−169.88 (15)
Ru1—Ru3—As1—C157.57 (6)C28—C29—C30—C311.8 (3)
Ru2—Ru3—As1—C174.74 (5)S1—C29—C30—C31−178.86 (14)
C54—Ru3—As1—C715.56 (8)C27—C26—C31—C30−1.1 (3)
C55—Ru3—As1—C7107.66 (7)As3—C26—C31—C30171.47 (14)
C53—Ru3—As1—C7−76.65 (7)C29—C30—C31—C26−0.8 (3)
Ru1—Ru3—As1—C7−173.80 (6)C26—As3—C32—C37−120.37 (13)
Ru2—Ru3—As1—C7−156.63 (6)C38—As3—C32—C37−18.14 (15)
C54—Ru3—As1—C13128.27 (7)Ru1—As3—C32—C37105.59 (13)
C55—Ru3—As1—C13−139.63 (7)C26—As3—C32—C3362.45 (14)
C53—Ru3—As1—C1336.06 (7)C38—As3—C32—C33164.68 (13)
Ru1—Ru3—As1—C13−61.09 (5)Ru1—As3—C32—C33−71.59 (14)
Ru2—Ru3—As1—C13−43.92 (5)C37—C32—C33—C340.4 (3)
C50—Ru2—As2—C20−78.97 (8)As3—C32—C33—C34177.68 (13)
C51—Ru2—As2—C2013.39 (7)C32—C33—C34—C35−1.7 (3)
C52—Ru2—As2—C20−171.19 (7)C33—C34—C35—C361.1 (3)
Ru3—Ru2—As2—C20106.79 (5)C33—C34—C35—S2−176.40 (14)
Ru1—Ru2—As2—C2077.75 (5)C45—S2—C35—C34−12.60 (18)
C50—Ru2—As2—C1438.70 (8)C45—S2—C35—C36169.84 (14)
C51—Ru2—As2—C14131.05 (7)C34—C35—C36—C370.7 (2)
C52—Ru2—As2—C14−53.52 (7)S2—C35—C36—C37178.44 (13)
Ru3—Ru2—As2—C14−135.55 (6)C35—C36—C37—C32−2.0 (2)
Ru1—Ru2—As2—C14−164.58 (6)C33—C32—C37—C361.4 (2)
C50—Ru2—As2—C13162.89 (8)As3—C32—C37—C36−175.82 (12)
C51—Ru2—As2—C13−104.76 (7)C26—As3—C38—C3920.61 (15)
C52—Ru2—As2—C1370.67 (7)C32—As3—C38—C39−83.30 (15)
Ru3—Ru2—As2—C13−11.35 (6)Ru1—As3—C38—C39151.38 (12)
Ru1—Ru2—As2—C13−40.39 (6)C26—As3—C38—C43−157.37 (14)
C49—Ru1—As3—C26168.10 (8)C32—As3—C38—C4398.72 (14)
C48—Ru1—As3—C2675.30 (8)Ru1—As3—C38—C43−26.59 (15)
C47—Ru1—As3—C26−98.77 (7)C43—C38—C39—C400.0 (3)
Ru3—Ru1—As3—C26−48.38 (7)As3—C38—C39—C40−178.00 (14)
Ru2—Ru1—As3—C260.78 (6)C38—C39—C40—C41−0.9 (3)
C49—Ru1—As3—C32−68.08 (8)C39—C40—C41—C421.1 (3)
C48—Ru1—As3—C32−160.87 (7)C39—C40—C41—S3−178.79 (14)
C47—Ru1—As3—C3225.06 (7)C46—S3—C41—C42−171.86 (15)
Ru3—Ru1—As3—C3275.45 (6)C46—S3—C41—C408.04 (18)
Ru2—Ru1—As3—C32124.61 (5)C40—C41—C42—C43−0.5 (3)
C49—Ru1—As3—C3849.87 (7)S3—C41—C42—C43179.43 (14)
C48—Ru1—As3—C38−42.92 (7)C41—C42—C43—C38−0.4 (3)
C47—Ru1—As3—C38143.01 (7)C39—C38—C43—C420.6 (3)
Ru3—Ru1—As3—C38−166.60 (6)As3—C38—C43—C42178.66 (14)
Ru2—Ru1—As3—C38−117.44 (5)

Symmetry codes: (i) −x+1, −y+1, −z.

Hydrogen-bond geometry (Å, °)

Cg1, Cg2, Cg3, Cg4 and Cg5 are the centroids of the C26–C31, C32–C37, C1–C6, C14–C19 and C38–C43 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C3—H3A···Cg1ii0.932.593.609 (2)134
C10—H10A···Cg2iii0.932.913.788 (2)156
C24—H24A···Cg3iv0.932.963.676 (2)136
C42—H42A···Cg4v0.932.813.641 (2)155
C46—H46C···Cg5vi0.962.903.742 (2)152

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: IS2586).

References

  • Bruce, M. I., Liddell, M. J., Hughes, C. A., Patrick, J. M., Skelton, B. W. & White, A. H. (1988). J. Organomet. Chem.347, 181–205.
  • Bruce, M. I., Liddell, M. J., Shawkataly, O. bin., Hughes, C. A., Skelton, B. W. & White, A. H. (1988). J. Organomet. Chem.347, 207–235.
  • Bruce, M. I., Matisons, J. G. & Nicholson, B. K. (1983). J. Organomet. Chem.247, 321–343.
  • Bruce, M. I., Shawkataly, O. bin. & Williams, M. L. (1985). J. Organomet. Chem.287, 127–131.
  • Bruker (2009). APEX2, SAINT and SADABS Bruker AXS Inc., Madison, Wisconsin, USA.
  • Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst.19, 105–107.
  • Shawkataly, O. bin, Khan, I. A., Sirat, S. S., Yeap, C. S. & Fun, H.-K. (2010a). Acta Cryst. E66, m1047–m1048. [PMC free article] [PubMed]
  • Shawkataly, O. bin, Khan, I. A., Sirat, S. S., Yeap, C. S. & Fun, H.-K. (2010b). Acta Cryst. E66, m1150–m1151. [PMC free article] [PubMed]
  • Shawkataly, O. bin, Khan, I. A., Yeap, C. S. & Fun, H.-K. (2010a). Acta Cryst. E66, m30–m31. [PMC free article] [PubMed]
  • Shawkataly, O. bin, Khan, I. A., Yeap, C. S. & Fun, H.-K. (2010b). Acta Cryst. E66, m180–m181. [PMC free article] [PubMed]
  • Shawkataly, O. bin, Ramalingam, K., Fun, H.-K., Abdul Rahman, A., & Razak, I. A. (2004). J. Cluster Sci.15, 387–394.
  • Shawkataly, O. bin, Ramalingam, K., Lee, S. T., Parameswary, M., Fun, H.-K. & Sivakumar, K. (1998). Polyhedron, 17, 1211–1216.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Spek, A. L. (2009). Acta Cryst. D65, 148–155. [PMC free article] [PubMed]

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