metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 1| January 2010| Pages m30-m31

Bis{[μ-bis­­(di­phenyl­phosphino)methane-1:2κ2P:P′]nona­carbonyl-1κ3C,2κ3C,3κ3C-[tris­­(4-meth­oxy­phen­yl)arsine-3κAs]-triangulo-triruthenium(0)} di­chloro­methane solvate

aChemical Sciences Programme, School of Distance Education, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia, and bX-ray Crystallography Unit, School of Physics, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia
*Correspondence e-mail: omarsa@usm.my

(Received 30 November 2009; accepted 3 December 2009; online 9 December 2009)

The asymmetric unit of the title triangulo-triruthenium compound, 2[Ru3(C21H21AsO3)(C25H22P2)(CO)9]·CH2Cl2, contains one triangulo-triruthenium complex mol­ecule and one half-mol­ecule of the dichloro­methane solvent. The dichloro­methane solvent lies across a crystallographic inversion center leading to the mol­ecule being disordered over two positions of equal occupancy. The bis­(diphenyl­phosphino)methane ligand bridges an Ru—Ru bond and the monodentate arsine ligand bonds to the third Ru atom. Both the arsine and phosphine ligands are equatorial with respect to the Ru3 triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three arsine-substituted benzene rings make dihedral angles of 82.00 (6), 76.67 (7) and 66.09 (6)° with each other. The dihedral angles between the two benzene rings are 80.12 (8) and 78.34 (7)° for the two diphenyl­phosphino groups. In the crystal packing, the mol­ecules are linked together into chains down the b axis via inter­molecular C—H⋯O hydrogen bonds. An inter­molecular C—H⋯O hydrogen bond and 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[Bruce, M. I., Shawkataly, O. bin & Williams, M. L. (1985). J. Organomet. Chem. 287, 127-131.], 1988a[Bruce, M. I., Liddell, M. J., Hughes, C. A., Patrick, J. M., Skelton, B. W. & White, A. H. (1988a). J. Organomet. Chem. 347, 181-205.],b[Bruce, M. I., Liddell, M. J., Shawkataly, O. bin, Hughes, C. A., Skelton, B. W. & White, A. H. (1988b). J. Organomet. Chem. 347, 207-235.]). For related structures, see: Shawkataly et al. (1998[Shawkataly, O. bin., Ramalingam, K., Lee, S. T., Parameswary, M., Fun, H.-K. & Sivakumar, K. (1998). Polyhedron, 17, 1211-1216.], 2004[Shawkataly, O. bin, Ramalingam, K., Fun, H.-K., Abdul Rahman, A., & Razak, I. A. (2004). J. Cluster Sci. 15, 387-394.], 2009[Shawkataly, O. bin, Khan, I. A., Yeap, C. S. & Fun, H.-K. (2009). Acta Cryst. E65, m1620-m1621.]). For the synthesis of tris­(4-methoxy­phen­yl)arsine, see: Blicke & Cataline (1938[Blicke, F. F. & Cataline, E. L. (1938). J. Am. Chem. Soc., 60, 419-422.]) and for that of μ-bis­(diphenylphosphino)methanedeca­carbonyl­tri­ruthenium(0), see: Bruce et al. (1983[Bruce, M. I., Matisons, J. G. & Nicholson, B. K. (1983). J. Organomet. Chem. 247, 321-343.]). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986[Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst. 19, 105-107.]).

[Scheme 1]

Experimental

Crystal data
  • 2[Ru3(C21H21AsO3)(C25H22P2)(CO)9]·CH2Cl2

  • Mr = 2756.85

  • Triclinic, [P \overline 1]

  • a = 10.7428 (1) Å

  • b = 12.6731 (1) Å

  • c = 20.6529 (2) Å

  • α = 95.523 (1)°

  • β = 101.315 (1)°

  • γ = 103.929 (1)°

  • V = 2645.47 (4) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 1.64 mm−1

  • T = 100 K

  • 0.30 × 0.23 × 0.14 mm

Data collection
  • Bruker SMART APEXII CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.637, Tmax = 0.797

  • 123575 measured reflections

  • 23203 independent reflections

  • 20247 reflections with I > 2σ(I)

  • Rint = 0.030

Refinement
  • R[F2 > 2σ(F2)] = 0.023

  • wR(F2) = 0.055

  • S = 1.02

  • 23203 reflections

  • 679 parameters

  • H-atom parameters constrained

  • Δρmax = 1.72 e Å−3

  • Δρmin = −1.34 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
C53—H53C⋯O2i 0.96 2.60 3.346 (2) 135
C56—H56A⋯O7 0.96 2.60 3.116 (3) 114
C22—H22ACg1ii 0.93 2.91 3.5901 (16) 131
C53—H53BCg2iii 0.96 2.85 3.6951 (17) 147
Symmetry codes: (i) x, y+1, z; (ii) x-1, y, z; (iii) -x+2, -y+2, -z+1. Cg1 and Cg2 are the centroids of theC32–C37 and C26–C31 benzene rings, respectively.

Data collection: APEX2 (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2005[Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL and PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]).

Supporting information


Comment top

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, 1988a,b). As part of our study of 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, 2009). Herein we report the synthesis and structure of the title compound.

The asymmetric 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 (symmetry code: 2 - x, 1 - y, -z) leading to disorder of this solvent molecule over two positions. The bond lengths and angles of title compound are comparable to those found in related structures (Shawkataly et al., 2009). The bis(diphenylphosphino)methane ligand bridges the Ru1—Ru2 bond and the monodentate arsine ligand bonds to the Ru3 atom. Both the arsine and phosphine 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 82.00 (6), 76.67 (7) and 66.09 (6)° with each other respectively. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 80.12 (8) and 78.34 (7)° for the two diphenylphosphino groups respectively.

In the crystal packing (Fig. 2), the molecules are linked together into chains via intermolecular C53—H53C···O2 contacts along the b axis. An intermolecular C56—H56A···O7 hydrogen bond and weak intermolecular C—H···π interactions further stabilize the crystal structure (Table 1).

Related literature top

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985, 1988a,b). For related structures, see: Shawkataly et al. (1998, 2004, 2009). For the synthesis of tris(4-methoxyphenyl)arsine, see: Blicke et al. (1938) and of bis(diphenylphosphino)methane, see: Bruce et al. (1983). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986).

Experimental top

The reactions were conducted under an atmosphere of high purity nitrogen using standard Schlenk techniques and hexane-dried over sodium metal. Tris(4-methoxyphenyl)arsine (Blicke et al., 1938) and µ-bis(diphenylphosphino)methanedecacarbonyltriruthenium(0) (Bruce et al., 1983) were prepared by reported procedures. The title compound was obtained by refluxing equimolar quantities of Ru3(CO)10(µ-Ph2PCH2PPh2) (102.4 mg, 0.1 mmol) and tris(4-methoxyphenyl)arsine (39.63 mg, 0.1 mmol) in hexane under a nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of CH3OH into CH2Cl2.

Refinement top

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). A rotating group model was applied for the methyl groups.

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT (Bruker, 2005); 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 structure of the title compound with 50% probability ellipsoids for non-H atoms. Atoms with suffix A are generated by the symmetry operation (2 - x, 1 - y, -z).
[Figure 2] Fig. 2. The crystal packing of the title compound, viewed down the a axis, showing the molecules linked along b axis. Hydrogen atoms that are not involved in the hydrogen-bonding (dashed lines) and solvent molecules have been omitted for clarity.
Bis{[µ-bis(diphenylphosphino)methane-1:2κ2P: P']nonacarbonyl-1κ3C,2κ3C,3κ3C- [tris(4-methoxyphenyl)arsine-3κAs]-triangulo-triruthenium(0)} dichloromethane solvate top
Crystal data top
2[Ru3(C21H21AsO3)(C25H22P2)(CO)9]·CH2Cl2Z = 1
Mr = 2756.85F(000) = 1370
Triclinic, P1Dx = 1.730 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.7428 (1) ÅCell parameters from 9697 reflections
b = 12.6731 (1) Åθ = 2.8–35.1°
c = 20.6529 (2) ŵ = 1.64 mm1
α = 95.523 (1)°T = 100 K
β = 101.315 (1)°Block, purple
γ = 103.929 (1)°0.30 × 0.23 × 0.14 mm
V = 2645.47 (4) Å3
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer
23203 independent reflections
Radiation source: fine-focus sealed tube20247 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
ϕ and ω scansθmax = 35.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2005)
h = 1717
Tmin = 0.637, Tmax = 0.797k = 2020
123575 measured reflectionsl = 3333
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)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.055H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0229P)2 + 1.6547P]
where P = (Fo2 + 2Fc2)/3
23203 reflections(Δ/σ)max = 0.003
679 parametersΔρmax = 1.72 e Å3
0 restraintsΔρmin = 1.34 e Å3
Crystal data top
2[Ru3(C21H21AsO3)(C25H22P2)(CO)9]·CH2Cl2γ = 103.929 (1)°
Mr = 2756.85V = 2645.47 (4) Å3
Triclinic, P1Z = 1
a = 10.7428 (1) ÅMo Kα radiation
b = 12.6731 (1) ŵ = 1.64 mm1
c = 20.6529 (2) ÅT = 100 K
α = 95.523 (1)°0.30 × 0.23 × 0.14 mm
β = 101.315 (1)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer
23203 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2005)
20247 reflections with I > 2σ(I)
Tmin = 0.637, Tmax = 0.797Rint = 0.030
123575 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0230 restraints
wR(F2) = 0.055H-atom parameters constrained
S = 1.02Δρmax = 1.72 e Å3
23203 reflectionsΔρmin = 1.34 e Å3
679 parameters
Special details top

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) top
xyzUiso*/UeqOcc. (<1)
Ru10.745666 (9)0.425733 (8)0.272810 (5)0.01139 (2)
Ru20.569657 (9)0.487278 (8)0.171185 (4)0.01062 (2)
Ru30.803319 (9)0.646604 (8)0.240008 (5)0.01147 (2)
As11.032151 (12)0.748971 (10)0.288763 (6)0.01240 (2)
P10.64526 (3)0.23960 (3)0.236633 (15)0.01201 (5)
P20.41178 (3)0.32412 (3)0.168781 (15)0.01140 (5)
O10.54704 (10)0.46246 (9)0.35615 (5)0.01989 (18)
O20.92704 (11)0.39895 (10)0.39911 (5)0.0257 (2)
O30.95575 (10)0.42132 (10)0.19116 (6)0.0241 (2)
O40.69735 (10)0.36155 (9)0.07987 (5)0.02031 (18)
O50.45036 (12)0.58679 (10)0.05376 (6)0.0284 (2)
O60.46711 (10)0.63687 (9)0.26185 (5)0.0227 (2)
O70.88918 (11)0.59722 (9)0.10904 (5)0.0227 (2)
O80.68903 (12)0.83005 (9)0.19351 (6)0.0267 (2)
O90.73330 (11)0.68897 (9)0.37569 (5)0.0252 (2)
O101.12273 (12)1.16961 (9)0.48187 (5)0.0266 (2)
O111.40724 (11)0.61008 (10)0.50258 (5)0.0236 (2)
O121.34237 (11)0.92350 (9)0.08579 (5)0.0238 (2)
C10.60776 (12)0.14917 (10)0.29888 (6)0.0155 (2)
C20.61938 (14)0.19130 (12)0.36533 (7)0.0200 (2)
H2A0.64340.26700.37880.024*
C30.59509 (17)0.12028 (14)0.41183 (8)0.0268 (3)
H3A0.60270.14880.45610.032*
C40.55954 (17)0.00719 (14)0.39210 (9)0.0297 (3)
H4A0.54400.03990.42320.036*
C50.54714 (17)0.03567 (13)0.32580 (9)0.0282 (3)
H5A0.52300.11140.31260.034*
C60.57086 (15)0.03478 (11)0.27945 (8)0.0220 (3)
H6A0.56220.00590.23520.026*
C70.74231 (12)0.16477 (10)0.19620 (6)0.0144 (2)
C80.86801 (13)0.16990 (12)0.23303 (7)0.0207 (2)
H8A0.89920.21220.27510.025*
C90.94680 (14)0.11242 (12)0.20732 (8)0.0245 (3)
H9A1.03020.11620.23230.029*
C100.90165 (14)0.04942 (12)0.14450 (8)0.0233 (3)
H10A0.95460.01100.12740.028*
C110.77749 (15)0.04389 (13)0.10737 (8)0.0246 (3)
H11A0.74730.00220.06510.030*
C120.69770 (14)0.10064 (12)0.13319 (7)0.0207 (2)
H12A0.61390.09580.10820.025*
C130.48897 (12)0.20925 (10)0.17294 (6)0.01391 (19)
H13A0.50570.18930.12950.017*
H13B0.42740.14620.18240.017*
C140.28467 (12)0.27167 (10)0.09186 (6)0.0140 (2)
C150.32348 (13)0.27282 (12)0.03100 (6)0.0189 (2)
H15A0.41170.30060.03070.023*
C160.23111 (15)0.23281 (13)0.02891 (7)0.0229 (3)
H16A0.25790.23280.06910.027*
C170.09873 (15)0.19283 (12)0.02904 (7)0.0231 (3)
H17A0.03680.16720.06920.028*
C180.05952 (14)0.19133 (13)0.03066 (8)0.0252 (3)
H18A0.02900.16410.03050.030*
C190.15155 (13)0.23028 (12)0.09126 (7)0.0206 (2)
H19A0.12420.22870.13130.025*
C200.32108 (12)0.31633 (10)0.23455 (6)0.01380 (19)
C210.25630 (12)0.39752 (11)0.24622 (6)0.0165 (2)
H21A0.25440.45060.21820.020*
C220.19488 (13)0.39905 (12)0.29952 (7)0.0202 (2)
H22A0.15280.45360.30720.024*
C230.19606 (14)0.31958 (14)0.34120 (7)0.0230 (3)
H23A0.15590.32130.37710.028*
C240.25741 (14)0.23753 (13)0.32909 (7)0.0222 (3)
H24A0.25710.18360.35660.027*
C250.31950 (12)0.23542 (11)0.27597 (6)0.0170 (2)
H25A0.36010.17990.26810.020*
C261.05575 (12)0.88441 (10)0.34835 (6)0.0149 (2)
C270.95099 (13)0.92839 (11)0.35364 (7)0.0183 (2)
H27A0.86790.89390.32690.022*
C280.96792 (14)1.02354 (11)0.39841 (7)0.0201 (2)
H28A0.89681.05200.40150.024*
C291.09228 (15)1.07508 (11)0.43817 (7)0.0190 (2)
C301.19835 (15)1.03087 (11)0.43365 (7)0.0213 (2)
H30A1.28131.06470.46080.026*
C311.18005 (13)0.93698 (11)0.38893 (7)0.0189 (2)
H31A1.25110.90850.38580.023*
C321.15368 (12)0.68892 (10)0.34692 (6)0.0140 (2)
C331.10840 (13)0.63630 (11)0.39765 (6)0.0167 (2)
H33A1.01900.61880.39720.020*
C341.19494 (14)0.60997 (12)0.44847 (7)0.0191 (2)
H34A1.16380.57550.48210.023*
C351.32949 (13)0.63521 (11)0.44929 (6)0.0176 (2)
C361.37556 (13)0.68384 (11)0.39775 (6)0.0173 (2)
H36A1.46430.69810.39710.021*
C371.28696 (13)0.71086 (11)0.34721 (7)0.0166 (2)
H37A1.31770.74420.31310.020*
C381.13298 (12)0.80171 (10)0.22457 (6)0.0145 (2)
C391.18482 (14)0.73120 (10)0.18772 (7)0.0176 (2)
H39A1.17140.65820.19440.021*
C401.25609 (14)0.76895 (11)0.14126 (7)0.0195 (2)
H40A1.29240.72200.11810.023*
C411.27291 (13)0.87730 (11)0.12957 (6)0.0172 (2)
C421.21673 (13)0.94699 (11)0.16395 (7)0.0170 (2)
H42A1.22451.01840.15480.020*
C431.14927 (12)0.90978 (10)0.21176 (6)0.0158 (2)
H43A1.11460.95730.23550.019*
C440.61781 (13)0.45018 (10)0.32303 (6)0.0154 (2)
C450.86226 (13)0.41157 (11)0.35056 (7)0.0173 (2)
C460.87634 (13)0.42870 (11)0.21981 (7)0.0173 (2)
C470.65515 (12)0.41014 (10)0.11587 (6)0.0150 (2)
C480.49368 (13)0.54928 (11)0.09827 (7)0.0171 (2)
C490.50943 (12)0.57944 (11)0.23128 (6)0.0161 (2)
C500.85260 (13)0.61005 (10)0.15679 (6)0.0164 (2)
C510.73810 (13)0.76296 (11)0.21037 (6)0.0172 (2)
C520.75643 (13)0.66540 (11)0.32505 (7)0.0177 (2)
C531.01782 (19)1.21524 (13)0.49108 (8)0.0299 (3)
H53A1.05251.28390.52070.045*
H53B0.95771.16520.51000.045*
H53C0.97241.22750.44880.045*
C541.54628 (15)0.63830 (14)0.50655 (8)0.0258 (3)
H54A1.59020.61650.54610.039*
H54B1.57820.71630.50830.039*
H54C1.56360.60100.46790.039*
C551.40600 (18)0.85522 (14)0.05196 (8)0.0302 (3)
H55A1.45530.89700.02450.045*
H55B1.34080.79340.02440.045*
H55C1.46450.82960.08430.045*
Cl10.88282 (6)0.50832 (5)0.04776 (3)0.04631 (12)
C561.0352 (3)0.5652 (2)0.00469 (16)0.0247 (5)0.50
H56A1.03440.63090.02230.030*0.50
H56B1.08770.58750.03610.030*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01110 (4)0.01066 (4)0.01140 (4)0.00242 (3)0.00058 (3)0.00214 (3)
Ru20.00987 (4)0.01158 (4)0.01061 (4)0.00317 (3)0.00215 (3)0.00225 (3)
Ru30.01149 (4)0.01044 (4)0.01217 (4)0.00238 (3)0.00266 (3)0.00171 (3)
As10.01191 (5)0.01124 (5)0.01406 (5)0.00301 (4)0.00338 (4)0.00119 (4)
P10.01127 (12)0.01126 (12)0.01308 (12)0.00303 (10)0.00155 (10)0.00214 (10)
P20.01008 (12)0.01277 (12)0.01112 (12)0.00306 (10)0.00179 (9)0.00197 (10)
O10.0203 (4)0.0230 (5)0.0168 (4)0.0054 (4)0.0056 (3)0.0029 (3)
O20.0234 (5)0.0291 (5)0.0211 (5)0.0048 (4)0.0027 (4)0.0092 (4)
O30.0196 (5)0.0311 (5)0.0276 (5)0.0119 (4)0.0094 (4)0.0126 (4)
O40.0191 (4)0.0240 (5)0.0181 (4)0.0076 (4)0.0047 (4)0.0011 (4)
O50.0297 (6)0.0364 (6)0.0242 (5)0.0152 (5)0.0046 (4)0.0154 (5)
O60.0209 (5)0.0241 (5)0.0250 (5)0.0086 (4)0.0085 (4)0.0008 (4)
O70.0276 (5)0.0223 (5)0.0198 (4)0.0059 (4)0.0102 (4)0.0029 (4)
O80.0343 (6)0.0234 (5)0.0278 (5)0.0160 (5)0.0071 (5)0.0086 (4)
O90.0283 (5)0.0246 (5)0.0196 (5)0.0005 (4)0.0099 (4)0.0018 (4)
O100.0374 (6)0.0177 (5)0.0217 (5)0.0076 (4)0.0035 (4)0.0054 (4)
O110.0220 (5)0.0315 (5)0.0177 (4)0.0100 (4)0.0005 (4)0.0071 (4)
O120.0273 (5)0.0229 (5)0.0234 (5)0.0034 (4)0.0135 (4)0.0064 (4)
C10.0132 (5)0.0152 (5)0.0178 (5)0.0030 (4)0.0026 (4)0.0054 (4)
C20.0221 (6)0.0189 (6)0.0187 (6)0.0040 (5)0.0042 (5)0.0058 (4)
C30.0313 (8)0.0284 (7)0.0205 (6)0.0045 (6)0.0063 (6)0.0104 (5)
C40.0332 (8)0.0267 (7)0.0303 (8)0.0035 (6)0.0096 (6)0.0162 (6)
C50.0326 (8)0.0175 (6)0.0340 (8)0.0021 (6)0.0090 (6)0.0101 (6)
C60.0247 (6)0.0156 (5)0.0249 (6)0.0024 (5)0.0065 (5)0.0052 (5)
C70.0132 (5)0.0124 (5)0.0182 (5)0.0040 (4)0.0038 (4)0.0028 (4)
C80.0153 (5)0.0195 (6)0.0256 (6)0.0071 (5)0.0004 (5)0.0015 (5)
C90.0147 (5)0.0211 (6)0.0369 (8)0.0082 (5)0.0019 (5)0.0007 (5)
C100.0202 (6)0.0187 (6)0.0335 (7)0.0085 (5)0.0094 (5)0.0016 (5)
C110.0250 (7)0.0256 (7)0.0243 (6)0.0124 (6)0.0044 (5)0.0024 (5)
C120.0195 (6)0.0232 (6)0.0199 (6)0.0105 (5)0.0017 (5)0.0011 (5)
C130.0128 (5)0.0126 (5)0.0150 (5)0.0034 (4)0.0008 (4)0.0002 (4)
C140.0133 (5)0.0142 (5)0.0133 (5)0.0029 (4)0.0010 (4)0.0018 (4)
C150.0168 (5)0.0245 (6)0.0146 (5)0.0058 (5)0.0021 (4)0.0012 (4)
C160.0248 (6)0.0285 (7)0.0138 (5)0.0082 (5)0.0009 (5)0.0001 (5)
C170.0224 (6)0.0228 (6)0.0179 (6)0.0039 (5)0.0054 (5)0.0012 (5)
C180.0157 (6)0.0306 (7)0.0225 (6)0.0011 (5)0.0026 (5)0.0030 (5)
C190.0137 (5)0.0266 (6)0.0180 (6)0.0006 (5)0.0012 (4)0.0040 (5)
C200.0110 (4)0.0169 (5)0.0126 (5)0.0025 (4)0.0019 (4)0.0025 (4)
C210.0145 (5)0.0190 (5)0.0170 (5)0.0051 (4)0.0047 (4)0.0030 (4)
C220.0146 (5)0.0260 (6)0.0194 (6)0.0050 (5)0.0051 (4)0.0011 (5)
C230.0162 (6)0.0363 (8)0.0158 (5)0.0043 (5)0.0057 (4)0.0035 (5)
C240.0182 (6)0.0309 (7)0.0177 (6)0.0036 (5)0.0053 (5)0.0103 (5)
C250.0136 (5)0.0202 (6)0.0174 (5)0.0037 (4)0.0035 (4)0.0061 (4)
C260.0159 (5)0.0130 (5)0.0155 (5)0.0035 (4)0.0037 (4)0.0011 (4)
C270.0168 (5)0.0173 (5)0.0201 (6)0.0046 (4)0.0041 (4)0.0008 (4)
C280.0226 (6)0.0169 (5)0.0224 (6)0.0065 (5)0.0082 (5)0.0004 (5)
C290.0279 (6)0.0135 (5)0.0154 (5)0.0049 (5)0.0061 (5)0.0011 (4)
C300.0226 (6)0.0159 (5)0.0213 (6)0.0035 (5)0.0004 (5)0.0009 (5)
C310.0178 (5)0.0146 (5)0.0223 (6)0.0044 (4)0.0015 (5)0.0002 (4)
C320.0139 (5)0.0133 (5)0.0153 (5)0.0041 (4)0.0037 (4)0.0020 (4)
C330.0163 (5)0.0177 (5)0.0163 (5)0.0036 (4)0.0050 (4)0.0023 (4)
C340.0199 (6)0.0227 (6)0.0159 (5)0.0050 (5)0.0063 (4)0.0050 (4)
C350.0188 (5)0.0189 (6)0.0144 (5)0.0061 (4)0.0017 (4)0.0013 (4)
C360.0155 (5)0.0195 (6)0.0176 (5)0.0061 (4)0.0034 (4)0.0033 (4)
C370.0157 (5)0.0176 (5)0.0185 (5)0.0058 (4)0.0059 (4)0.0044 (4)
C380.0141 (5)0.0135 (5)0.0155 (5)0.0028 (4)0.0039 (4)0.0024 (4)
C390.0220 (6)0.0132 (5)0.0190 (5)0.0040 (4)0.0081 (5)0.0031 (4)
C400.0225 (6)0.0172 (5)0.0203 (6)0.0049 (5)0.0090 (5)0.0020 (4)
C410.0159 (5)0.0181 (5)0.0160 (5)0.0011 (4)0.0040 (4)0.0024 (4)
C420.0166 (5)0.0150 (5)0.0186 (5)0.0023 (4)0.0035 (4)0.0043 (4)
C430.0148 (5)0.0139 (5)0.0190 (5)0.0042 (4)0.0043 (4)0.0024 (4)
C440.0160 (5)0.0139 (5)0.0144 (5)0.0028 (4)0.0002 (4)0.0023 (4)
C450.0164 (5)0.0156 (5)0.0187 (5)0.0027 (4)0.0021 (4)0.0042 (4)
C460.0149 (5)0.0178 (5)0.0187 (5)0.0042 (4)0.0010 (4)0.0063 (4)
C470.0119 (5)0.0164 (5)0.0156 (5)0.0026 (4)0.0017 (4)0.0030 (4)
C480.0157 (5)0.0187 (5)0.0179 (5)0.0055 (4)0.0043 (4)0.0044 (4)
C490.0148 (5)0.0175 (5)0.0160 (5)0.0041 (4)0.0034 (4)0.0036 (4)
C500.0175 (5)0.0132 (5)0.0182 (5)0.0037 (4)0.0036 (4)0.0023 (4)
C510.0181 (5)0.0171 (5)0.0166 (5)0.0042 (4)0.0052 (4)0.0019 (4)
C520.0162 (5)0.0166 (5)0.0178 (5)0.0004 (4)0.0035 (4)0.0017 (4)
C530.0457 (10)0.0229 (7)0.0245 (7)0.0160 (7)0.0098 (7)0.0016 (5)
C540.0207 (6)0.0306 (7)0.0235 (7)0.0081 (6)0.0024 (5)0.0035 (6)
C550.0376 (9)0.0287 (7)0.0267 (7)0.0046 (6)0.0191 (7)0.0027 (6)
Cl10.0587 (3)0.0458 (3)0.0360 (2)0.0284 (2)0.0026 (2)0.00689 (19)
C560.0269 (14)0.0214 (12)0.0279 (14)0.0061 (11)0.0127 (11)0.0010 (10)
Geometric parameters (Å, º) top
Ru1—C451.8852 (13)C15—C161.3886 (19)
Ru1—C461.9379 (14)C15—H15A0.9300
Ru1—C441.9391 (13)C16—C171.389 (2)
Ru1—P12.3250 (3)C16—H16A0.9300
Ru1—Ru22.8384 (1)C17—C181.379 (2)
Ru1—Ru32.8936 (1)C17—H17A0.9300
Ru2—C481.8988 (13)C18—C191.3958 (19)
Ru2—C491.9295 (13)C18—H18A0.9300
Ru2—C471.9322 (13)C19—H19A0.9300
Ru2—P22.3266 (3)C20—C251.3963 (17)
Ru2—Ru32.8294 (1)C20—C211.4014 (18)
Ru3—C511.8822 (13)C21—C221.3909 (18)
Ru3—C521.9286 (13)C21—H21A0.9300
Ru3—C501.9417 (13)C22—C231.387 (2)
Ru3—As12.4458 (2)C22—H22A0.9300
As1—C381.9399 (12)C23—C241.387 (2)
As1—C321.9405 (12)C23—H23A0.9300
As1—C261.9458 (12)C24—C251.3926 (19)
P1—C71.8300 (12)C24—H24A0.9300
P1—C11.8421 (13)C25—H25A0.9300
P1—C131.8499 (12)C26—C271.3884 (18)
P2—C201.8175 (12)C26—C311.3980 (18)
P2—C141.8272 (12)C27—C281.3984 (18)
P2—C131.8416 (12)C27—H27A0.9300
O1—C441.1449 (16)C28—C291.390 (2)
O2—C451.1515 (16)C28—H28A0.9300
O3—C461.1457 (17)C29—C301.400 (2)
O4—C471.1473 (15)C30—C311.3827 (19)
O5—C481.1446 (16)C30—H30A0.9300
O6—C491.1483 (16)C31—H31A0.9300
O7—C501.1427 (16)C32—C371.3900 (17)
O8—C511.1502 (17)C32—C331.3991 (17)
O9—C521.1500 (16)C33—C341.3824 (19)
O10—C291.3580 (16)C33—H33A0.9300
O10—C531.420 (2)C34—C351.3995 (19)
O11—C351.3584 (16)C34—H34A0.9300
O11—C541.4335 (19)C35—C361.3943 (18)
O12—C411.3689 (16)C36—C371.3958 (18)
O12—C551.4353 (19)C36—H36A0.9300
C1—C21.3940 (19)C37—H37A0.9300
C1—C61.4031 (19)C38—C431.3960 (17)
C2—C31.397 (2)C38—C391.4010 (17)
C2—H2A0.9300C39—C401.3914 (18)
C3—C41.389 (2)C39—H39A0.9300
C3—H3A0.9300C40—C411.3922 (19)
C4—C51.392 (2)C40—H40A0.9300
C4—H4A0.9300C41—C421.3973 (19)
C5—C61.389 (2)C42—C431.3886 (18)
C5—H5A0.9300C42—H42A0.9300
C6—H6A0.9300C43—H43A0.9300
C7—C121.3956 (18)C53—H53A0.9600
C7—C81.3969 (18)C53—H53B0.9600
C8—C91.3884 (19)C53—H53C0.9600
C8—H8A0.9300C54—H54A0.9600
C9—C101.387 (2)C54—H54B0.9600
C9—H9A0.9300C54—H54C0.9600
C10—C111.384 (2)C55—H55A0.9600
C10—H10A0.9300C55—H55B0.9600
C11—C121.3925 (19)C55—H55C0.9600
C11—H11A0.9300Cl1—C561.651 (3)
C12—H12A0.9300Cl1—C56i1.741 (3)
C13—H13A0.9700C56—C56i1.689 (6)
C13—H13B0.9700C56—Cl1i1.741 (3)
C14—C191.3969 (18)C56—H56A0.9600
C14—C151.4000 (18)C56—H56B0.9602
C45—Ru1—C4692.43 (6)C18—C17—H17A120.1
C45—Ru1—C4491.81 (5)C16—C17—H17A120.1
C46—Ru1—C44169.56 (5)C17—C18—C19120.60 (14)
C45—Ru1—P197.70 (4)C17—C18—H18A119.7
C46—Ru1—P193.18 (4)C19—C18—H18A119.7
C44—Ru1—P195.70 (4)C18—C19—C14120.04 (13)
C45—Ru1—Ru2168.35 (4)C18—C19—H19A120.0
C46—Ru1—Ru293.26 (4)C14—C19—H19A120.0
C44—Ru1—Ru280.96 (4)C25—C20—C21118.98 (11)
P1—Ru1—Ru292.128 (8)C25—C20—P2122.11 (10)
C45—Ru1—Ru3112.70 (4)C21—C20—P2118.83 (9)
C46—Ru1—Ru375.74 (4)C22—C21—C20120.29 (12)
C44—Ru1—Ru393.83 (4)C22—C21—H21A119.9
P1—Ru1—Ru3147.777 (9)C20—C21—H21A119.9
Ru2—Ru1—Ru359.149 (3)C23—C22—C21120.30 (13)
C48—Ru2—C4989.82 (5)C23—C22—H22A119.8
C48—Ru2—C4792.03 (5)C21—C22—H22A119.8
C49—Ru2—C47171.56 (5)C24—C23—C22119.75 (13)
C48—Ru2—P2103.83 (4)C24—C23—H23A120.1
C49—Ru2—P297.23 (4)C22—C23—H23A120.1
C47—Ru2—P290.32 (4)C23—C24—C25120.39 (13)
C48—Ru2—Ru3106.51 (4)C23—C24—H24A119.8
C49—Ru2—Ru376.49 (4)C25—C24—H24A119.8
C47—Ru2—Ru395.10 (4)C24—C25—C20120.25 (13)
P2—Ru2—Ru3148.940 (9)C24—C25—H25A119.9
C48—Ru2—Ru1164.95 (4)C20—C25—H25A119.9
C49—Ru2—Ru195.44 (4)C27—C26—C31118.76 (12)
C47—Ru2—Ru180.81 (4)C27—C26—As1121.69 (10)
P2—Ru2—Ru189.521 (8)C31—C26—As1119.50 (9)
Ru3—Ru2—Ru161.397 (3)C26—C27—C28121.30 (13)
C51—Ru3—C5293.26 (6)C26—C27—H27A119.3
C51—Ru3—C5093.52 (5)C28—C27—H27A119.3
C52—Ru3—C50172.95 (5)C29—C28—C27119.21 (13)
C51—Ru3—As198.90 (4)C29—C28—H28A120.4
C52—Ru3—As191.63 (4)C27—C28—H28A120.4
C50—Ru3—As189.25 (4)O10—C29—C28125.03 (13)
C51—Ru3—Ru292.28 (4)O10—C29—C30115.01 (13)
C52—Ru3—Ru297.53 (4)C28—C29—C30119.95 (12)
C50—Ru3—Ru280.25 (4)C31—C30—C29120.11 (13)
As1—Ru3—Ru2165.117 (5)C31—C30—H30A119.9
C51—Ru3—Ru1147.69 (4)C29—C30—H30A119.9
C52—Ru3—Ru176.85 (4)C30—C31—C26120.66 (13)
C50—Ru3—Ru196.33 (4)C30—C31—H31A119.7
As1—Ru3—Ru1111.900 (5)C26—C31—H31A119.7
Ru2—Ru3—Ru159.454 (3)C37—C32—C33118.73 (12)
C38—As1—C32102.09 (5)C37—C32—As1123.00 (9)
C38—As1—C26101.52 (5)C33—C32—As1117.45 (9)
C32—As1—C2697.20 (5)C34—C33—C32120.79 (12)
C38—As1—Ru3114.76 (4)C34—C33—H33A119.6
C32—As1—Ru3122.65 (4)C32—C33—H33A119.6
C26—As1—Ru3115.26 (4)C33—C34—C35119.99 (12)
C7—P1—C198.79 (6)C33—C34—H34A120.0
C7—P1—C13102.47 (6)C35—C34—H34A120.0
C1—P1—C13104.49 (6)O11—C35—C36124.43 (12)
C7—P1—Ru1115.03 (4)O11—C35—C34115.63 (12)
C1—P1—Ru1118.96 (4)C36—C35—C34119.94 (12)
C13—P1—Ru1114.70 (4)C35—C36—C37119.25 (12)
C20—P2—C14104.26 (6)C35—C36—H36A120.4
C20—P2—C13105.29 (6)C37—C36—H36A120.4
C14—P2—C1399.97 (6)C32—C37—C36121.23 (12)
C20—P2—Ru2117.87 (4)C32—C37—H37A119.4
C14—P2—Ru2117.41 (4)C36—C37—H37A119.4
C13—P2—Ru2109.99 (4)C43—C38—C39118.67 (11)
C29—O10—C53117.49 (13)C43—C38—As1120.24 (9)
C35—O11—C54117.37 (11)C39—C38—As1121.00 (9)
C41—O12—C55116.68 (12)C40—C39—C38120.91 (12)
C2—C1—C6119.10 (12)C40—C39—H39A119.5
C2—C1—P1121.73 (10)C38—C39—H39A119.5
C6—C1—P1119.13 (10)C39—C40—C41119.75 (12)
C1—C2—C3120.26 (13)C39—C40—H40A120.1
C1—C2—H2A119.9C41—C40—H40A120.1
C3—C2—H2A119.9O12—C41—C40124.72 (12)
C4—C3—C2120.12 (15)O12—C41—C42115.49 (12)
C4—C3—H3A119.9C40—C41—C42119.78 (12)
C2—C3—H3A119.9C43—C42—C41120.12 (12)
C3—C4—C5120.04 (14)C43—C42—H42A119.9
C3—C4—H4A120.0C41—C42—H42A119.9
C5—C4—H4A120.0C42—C43—C38120.67 (12)
C6—C5—C4119.93 (14)C42—C43—H43A119.7
C6—C5—H5A120.0C38—C43—H43A119.7
C4—C5—H5A120.0O1—C44—Ru1175.51 (11)
C5—C6—C1120.54 (14)O2—C45—Ru1175.86 (12)
C5—C6—H6A119.7O3—C46—Ru1173.10 (12)
C1—C6—H6A119.7O4—C47—Ru2175.10 (11)
C12—C7—C8118.63 (12)O5—C48—Ru2178.46 (12)
C12—C7—P1124.75 (10)O6—C49—Ru2173.63 (12)
C8—C7—P1116.57 (10)O7—C50—Ru3174.12 (12)
C9—C8—C7120.57 (13)O8—C51—Ru3174.56 (12)
C9—C8—H8A119.7O9—C52—Ru3172.38 (12)
C7—C8—H8A119.7O10—C53—H53A109.5
C10—C9—C8120.28 (13)O10—C53—H53B109.5
C10—C9—H9A119.9H53A—C53—H53B109.5
C8—C9—H9A119.9O10—C53—H53C109.5
C11—C10—C9119.77 (13)H53A—C53—H53C109.5
C11—C10—H10A120.1H53B—C53—H53C109.5
C9—C10—H10A120.1O11—C54—H54A109.5
C10—C11—C12120.14 (14)O11—C54—H54B109.5
C10—C11—H11A119.9H54A—C54—H54B109.5
C12—C11—H11A119.9O11—C54—H54C109.5
C11—C12—C7120.60 (13)H54A—C54—H54C109.5
C11—C12—H12A119.7H54B—C54—H54C109.5
C7—C12—H12A119.7O12—C55—H55A109.5
P2—C13—P1114.19 (6)O12—C55—H55B109.5
P2—C13—H13A108.7H55A—C55—H55B109.5
P1—C13—H13A108.7O12—C55—H55C109.5
P2—C13—H13B108.7H55A—C55—H55C109.5
P1—C13—H13B108.7H55B—C55—H55C109.5
H13A—C13—H13B107.6C56—Cl1—C56i59.66 (18)
C19—C14—C15118.92 (12)Cl1—C56—C56i62.8 (2)
C19—C14—P2122.99 (10)Cl1—C56—Cl1i120.34 (18)
C15—C14—P2118.08 (9)C56i—C56—Cl1i57.53 (19)
C16—C15—C14120.45 (13)Cl1—C56—H56A107.2
C16—C15—H15A119.8C56i—C56—H56A126.2
C14—C15—H15A119.8Cl1i—C56—H56A107.0
C15—C16—C17120.21 (13)Cl1—C56—H56B107.3
C15—C16—H16A119.9C56i—C56—H56B126.8
C17—C16—H16A119.9Cl1i—C56—H56B107.4
C18—C17—C16119.76 (13)H56A—C56—H56B107.0
C45—Ru1—Ru2—C4886.4 (3)C7—P1—C1—C2134.94 (11)
C46—Ru1—Ru2—C4832.64 (16)C13—P1—C1—C2119.66 (11)
C44—Ru1—Ru2—C48138.62 (16)Ru1—P1—C1—C29.85 (13)
P1—Ru1—Ru2—C48125.95 (16)C7—P1—C1—C642.85 (12)
Ru3—Ru1—Ru2—C4838.61 (16)C13—P1—C1—C662.56 (12)
C45—Ru1—Ru2—C4923.6 (2)Ru1—P1—C1—C6167.94 (9)
C46—Ru1—Ru2—C49142.63 (6)C6—C1—C2—C30.3 (2)
C44—Ru1—Ru2—C4928.62 (5)P1—C1—C2—C3177.51 (12)
P1—Ru1—Ru2—C49124.06 (4)C1—C2—C3—C40.2 (2)
Ru3—Ru1—Ru2—C4971.38 (4)C2—C3—C4—C50.4 (3)
C45—Ru1—Ru2—C47148.8 (2)C3—C4—C5—C60.2 (3)
C46—Ru1—Ru2—C4729.75 (5)C4—C5—C6—C10.2 (2)
C44—Ru1—Ru2—C47159.00 (5)C2—C1—C6—C50.5 (2)
P1—Ru1—Ru2—C4763.56 (4)P1—C1—C6—C5177.38 (12)
Ru3—Ru1—Ru2—C47101.00 (4)C1—P1—C7—C12105.58 (12)
C45—Ru1—Ru2—P2120.8 (2)C13—P1—C7—C121.49 (13)
C46—Ru1—Ru2—P2120.14 (4)Ru1—P1—C7—C12126.62 (11)
C44—Ru1—Ru2—P268.60 (4)C1—P1—C7—C871.82 (11)
P1—Ru1—Ru2—P226.836 (11)C13—P1—C7—C8178.89 (10)
Ru3—Ru1—Ru2—P2168.606 (8)Ru1—P1—C7—C855.97 (11)
C45—Ru1—Ru2—Ru347.8 (2)C12—C7—C8—C90.1 (2)
C46—Ru1—Ru2—Ru371.25 (4)P1—C7—C8—C9177.66 (12)
C44—Ru1—Ru2—Ru3100.01 (4)C7—C8—C9—C100.2 (2)
P1—Ru1—Ru2—Ru3164.558 (9)C8—C9—C10—C110.0 (2)
C48—Ru2—Ru3—C5126.29 (6)C9—C10—C11—C120.5 (2)
C49—Ru2—Ru3—C5159.44 (5)C10—C11—C12—C70.9 (2)
C47—Ru2—Ru3—C51119.93 (5)C8—C7—C12—C110.6 (2)
P2—Ru2—Ru3—C51140.93 (4)P1—C7—C12—C11178.00 (12)
Ru1—Ru2—Ru3—C51163.44 (4)C20—P2—C13—P182.77 (8)
C48—Ru2—Ru3—C52119.88 (6)C14—P2—C13—P1169.33 (7)
C49—Ru2—Ru3—C5234.16 (6)Ru2—P2—C13—P145.19 (7)
C47—Ru2—Ru3—C52146.48 (6)C7—P1—C13—P2144.34 (7)
P2—Ru2—Ru3—C5247.34 (4)C1—P1—C13—P2113.03 (7)
Ru1—Ru2—Ru3—C5269.85 (4)Ru1—P1—C13—P218.98 (8)
C48—Ru2—Ru3—C5066.89 (6)C20—P2—C14—C193.77 (13)
C49—Ru2—Ru3—C50152.61 (5)C13—P2—C14—C19104.96 (12)
C47—Ru2—Ru3—C5026.75 (5)Ru2—P2—C14—C19136.22 (10)
P2—Ru2—Ru3—C50125.89 (4)C20—P2—C14—C15176.58 (10)
Ru1—Ru2—Ru3—C50103.38 (4)C13—P2—C14—C1574.70 (11)
C48—Ru2—Ru3—As1112.57 (5)Ru2—P2—C14—C1544.12 (11)
C49—Ru2—Ru3—As1161.71 (4)C19—C14—C15—C160.4 (2)
C47—Ru2—Ru3—As118.93 (4)P2—C14—C15—C16179.29 (11)
P2—Ru2—Ru3—As180.21 (3)C14—C15—C16—C171.0 (2)
Ru1—Ru2—Ru3—As157.70 (2)C15—C16—C17—C181.1 (2)
C48—Ru2—Ru3—Ru1170.27 (4)C16—C17—C18—C190.4 (2)
C49—Ru2—Ru3—Ru1104.01 (4)C17—C18—C19—C140.3 (2)
C47—Ru2—Ru3—Ru176.63 (4)C15—C14—C19—C180.3 (2)
P2—Ru2—Ru3—Ru122.512 (16)P2—C14—C19—C18179.92 (12)
C45—Ru1—Ru3—C51138.48 (9)C14—P2—C20—C25104.89 (11)
C46—Ru1—Ru3—C51134.90 (8)C13—P2—C20—C250.13 (12)
C44—Ru1—Ru3—C5144.91 (8)Ru2—P2—C20—C25122.92 (10)
P1—Ru1—Ru3—C5162.12 (8)C14—P2—C20—C2178.47 (11)
Ru2—Ru1—Ru3—C5132.18 (7)C13—P2—C20—C21176.78 (10)
C45—Ru1—Ru3—C5263.56 (6)Ru2—P2—C20—C2153.72 (11)
C46—Ru1—Ru3—C52150.17 (6)C25—C20—C21—C221.89 (19)
C44—Ru1—Ru3—C5230.01 (5)P2—C20—C21—C22174.86 (10)
P1—Ru1—Ru3—C52137.04 (4)C20—C21—C22—C230.6 (2)
Ru2—Ru1—Ru3—C52107.11 (4)C21—C22—C23—C240.8 (2)
C45—Ru1—Ru3—C50114.61 (6)C22—C23—C24—C251.0 (2)
C46—Ru1—Ru3—C5027.99 (6)C23—C24—C25—C200.3 (2)
C44—Ru1—Ru3—C50151.82 (5)C21—C20—C25—C241.72 (19)
P1—Ru1—Ru3—C5044.79 (4)P2—C20—C25—C24174.92 (10)
Ru2—Ru1—Ru3—C5074.73 (4)C38—As1—C26—C27114.32 (11)
C45—Ru1—Ru3—As122.87 (5)C32—As1—C26—C27141.72 (11)
C46—Ru1—Ru3—As163.75 (4)Ru3—As1—C26—C2710.35 (12)
C44—Ru1—Ru3—As1116.44 (4)C38—As1—C26—C3168.20 (11)
P1—Ru1—Ru3—As1136.533 (16)C32—As1—C26—C3135.76 (11)
Ru2—Ru1—Ru3—As1166.468 (6)Ru3—As1—C26—C31167.14 (9)
C45—Ru1—Ru3—Ru2170.66 (4)C31—C26—C27—C280.1 (2)
C46—Ru1—Ru3—Ru2102.72 (4)As1—C26—C27—C28177.59 (10)
C44—Ru1—Ru3—Ru277.09 (4)C26—C27—C28—C290.2 (2)
P1—Ru1—Ru3—Ru229.935 (16)C53—O10—C29—C284.6 (2)
C51—Ru3—As1—C3868.91 (6)C53—O10—C29—C30176.87 (13)
C52—Ru3—As1—C38162.47 (6)C27—C28—C29—O10177.70 (13)
C50—Ru3—As1—C3824.53 (5)C27—C28—C29—C300.8 (2)
Ru2—Ru3—As1—C3869.37 (5)O10—C29—C30—C31177.59 (13)
Ru1—Ru3—As1—C38121.05 (4)C28—C29—C30—C311.0 (2)
C51—Ru3—As1—C32166.36 (6)C29—C30—C31—C260.7 (2)
C52—Ru3—As1—C3272.81 (6)C27—C26—C31—C300.2 (2)
C50—Ru3—As1—C32100.20 (6)As1—C26—C31—C30177.39 (11)
Ru2—Ru3—As1—C3255.36 (5)C38—As1—C32—C3714.58 (12)
Ru1—Ru3—As1—C323.67 (4)C26—As1—C32—C3788.89 (11)
C51—Ru3—As1—C2648.52 (6)Ru3—As1—C32—C37144.83 (9)
C52—Ru3—As1—C2645.03 (6)C38—As1—C32—C33175.94 (10)
C50—Ru3—As1—C26141.96 (6)C26—As1—C32—C3380.59 (10)
Ru2—Ru3—As1—C26173.19 (4)Ru3—As1—C32—C3345.69 (11)
Ru1—Ru3—As1—C26121.51 (4)C37—C32—C33—C342.24 (19)
C45—Ru1—P1—C777.49 (6)As1—C32—C33—C34167.71 (10)
C46—Ru1—P1—C715.39 (6)C32—C33—C34—C350.5 (2)
C44—Ru1—P1—C7170.10 (6)C54—O11—C35—C361.7 (2)
Ru2—Ru1—P1—C7108.77 (5)C54—O11—C35—C34177.78 (13)
Ru3—Ru1—P1—C783.39 (5)C33—C34—C35—O11177.50 (12)
C45—Ru1—P1—C139.32 (6)C33—C34—C35—C362.0 (2)
C46—Ru1—P1—C1132.20 (6)O11—C35—C36—C37176.82 (13)
C44—Ru1—P1—C153.29 (6)C34—C35—C36—C372.6 (2)
Ru2—Ru1—P1—C1134.41 (5)C33—C32—C37—C361.58 (19)
Ru3—Ru1—P1—C1159.80 (5)As1—C32—C37—C36167.77 (10)
C45—Ru1—P1—C13164.01 (6)C35—C36—C37—C320.8 (2)
C46—Ru1—P1—C13103.11 (6)C32—As1—C38—C43127.57 (10)
C44—Ru1—P1—C1371.40 (6)C26—As1—C38—C4327.52 (11)
Ru2—Ru1—P1—C139.72 (4)Ru3—As1—C38—C4397.48 (10)
Ru3—Ru1—P1—C1335.11 (5)C32—As1—C38—C3955.80 (11)
C48—Ru2—P2—C20109.00 (6)C26—As1—C38—C39155.86 (11)
C49—Ru2—P2—C2017.40 (6)Ru3—As1—C38—C3979.15 (11)
C47—Ru2—P2—C20158.83 (6)C43—C38—C39—C402.7 (2)
Ru3—Ru2—P2—C2058.38 (5)As1—C38—C39—C40179.41 (11)
Ru1—Ru2—P2—C2078.02 (5)C38—C39—C40—C412.0 (2)
C48—Ru2—P2—C1417.01 (6)C55—O12—C41—C402.6 (2)
C49—Ru2—P2—C14108.61 (6)C55—O12—C41—C42177.35 (13)
C47—Ru2—P2—C1475.16 (6)C39—C40—C41—O12179.11 (13)
Ru3—Ru2—P2—C14175.61 (4)C39—C40—C41—C420.8 (2)
Ru1—Ru2—P2—C14155.96 (5)O12—C41—C42—C43177.09 (12)
C48—Ru2—P2—C13130.35 (6)C40—C41—C42—C432.8 (2)
C49—Ru2—P2—C13138.05 (6)C41—C42—C43—C382.08 (19)
C47—Ru2—P2—C1338.18 (6)C39—C38—C43—C420.68 (19)
Ru3—Ru2—P2—C1362.27 (5)As1—C38—C43—C42177.38 (10)
Ru1—Ru2—P2—C1342.63 (4)C56i—Cl1—C56—Cl1i0.0
Symmetry code: (i) x+2, y+1, z.
Hydrogen-bond geometry (Å, º) top
Cg1 and Cg2 are the centroids of theC32–C37 and C26–C31 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C53—H53C···O2ii0.962.603.346 (2)135
C56—H56A···O70.962.603.116 (3)114
C22—H22A···Cg1iii0.932.913.5901 (16)131
C53—H53B···Cg2iv0.962.853.6951 (17)147
Symmetry codes: (ii) x, y+1, z; (iii) x1, y, z; (iv) x+2, y+2, z+1.

Experimental details

Crystal data
Chemical formula2[Ru3(C21H21AsO3)(C25H22P2)(CO)9]·CH2Cl2
Mr2756.85
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)10.7428 (1), 12.6731 (1), 20.6529 (2)
α, β, γ (°)95.523 (1), 101.315 (1), 103.929 (1)
V3)2645.47 (4)
Z1
Radiation typeMo Kα
µ (mm1)1.64
Crystal size (mm)0.30 × 0.23 × 0.14
Data collection
DiffractometerBruker SMART APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2005)
Tmin, Tmax0.637, 0.797
No. of measured, independent and
observed [I > 2σ(I)] reflections
123575, 23203, 20247
Rint0.030
(sin θ/λ)max1)0.807
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.055, 1.02
No. of reflections23203
No. of parameters679
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.72, 1.34

Computer programs: APEX2 (Bruker, 2005), SAINT (Bruker, 2005), SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009).

Hydrogen-bond geometry (Å, º) top
Cg1 and Cg2 are the centroids of theC32–C37 and C26–C31 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C53—H53C···O2i0.96002.60003.346 (2)135.00
C56—H56A···O70.96002.60003.116 (3)114.00
C22—H22A···Cg1ii0.93002.91003.5901 (16)131.00
C53—H53B···Cg2iii0.96002.85003.6951 (17)147.00
Symmetry codes: (i) x, y+1, z; (ii) x1, y, z; (iii) x+2, y+2, z+1.
 

Footnotes

On secondment to: Multimedia University, Melaka Campus, Jalan Ayer Keroh Lama, 74750 Melaka, Malaysia.

§Thomson Reuters ResearcherID: A-5523-2009.

Thomson Reuters ResearcherID: A-3561-2009. Additional correspondence author, e-mail: hkfun@usm.my.

Acknowledgements

The authors would like to thank the Malaysian Government and Universiti Sains Malaysia (USM) for the Research grant 1001/PJJAUH/811115. IAK is grateful to USM for a 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.

References

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Volume 66| Part 1| January 2010| Pages m30-m31
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