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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 2| February 2010| Pages m176-m177
https://doi.org/10.1107/S1600536809055275

[μ-Bis(di­phenyl­arsino)methane-1:2κ2As:As′]nona­carbonyl-1κ3C,2κ3C,3κ3C-[(penta­fluoro­phen­yl)di­phenyl­phosphine-3κP]-triangulo-triruthenium(0) chloro­form monosolvate

Omar bin Shawkataly,a*‡ Imthyaz Ahmed Khan,a Chin Sing Yeapb§ and Hoong-Kun Funb

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 10 December 2009; accepted 23 December 2009; online 16 January 2010)

The asymmetric unit of the title triangulo-triruthenium compound, [Ru3(C25H22As2)(C18H10F5P)(CO)9]·CHCl3, contains one mol­ecule of the triangulo-triruthenium complex and one mol­ecule of the disordered chloro­form solvent. The bis­(diphenyl­arsino)methane ligand bridges an Ru—Ru bond and the monodentate phosphine 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 phosphine-substituted benzene rings make dihedral angles of 68.43 (15), 65.14 (14) and 89.75 (14)° with each other. The dihedral angles between the two benzene rings are 80.70 (15) and 84.53 (16)° for the two diphenyl­arsino groups. In the crystal packing, the mol­ecules are linked into a plane parallel to bc by inter­molecular C—H⋯O and C—H⋯F hydrogen bonds. 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 μ-bis­(diphenyl­arsino)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

  • [Ru3(C25H22As2)(C18H10F5P)(CO)9]·CHCl3

  • Mr = 1499.16

  • Triclinic, [P \overline 1]

  • a = 12.6354 (3) Å

  • b = 14.1572 (3) Å

  • c = 16.2418 (4) Å

  • α = 81.497 (1)°

  • β = 81.452 (1)°

  • γ = 74.994 (1)°

  • V = 2756.86 (11) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.25 mm−1

  • T = 100 K

  • 0.46 × 0.20 × 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 = 0.427, Tmax = 0.745

  • 83481 measured reflections

  • 15949 independent reflections

  • 13916 reflections with I > 2σ(I)

  • Rint = 0.028
Refinement

  • R[F2 > 2σ(F2)] = 0.032

  • wR(F2) = 0.088

  • S = 1.07

  • 15949 reflections

  • 702 parameters

  • 6 restraints

  • H-atom parameters constrained

  • Δρmax = 2.05 e Å−3

  • Δρmin = −1.70 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1 and Cg2 are the centroids of the C1–C6 and C32–C37 benzene rings, respectively.
D—H⋯A D—H H⋯A D⋯A D—H⋯A
C10—H10A⋯O5i 0.93 2.58 3.469 (4) 160
C12—H12A⋯F2ii 0.93 2.48 3.274 (3) 143
C22—H22A⋯O4iii 0.93 2.59 3.451 (5) 154
C34—H34A⋯O4iv 0.93 2.49 3.201 (4) 134
C39—H39A⋯Cg1v 0.93 2.93 3.749 (3) 148
C41—H41A⋯Cg2vi 0.93 2.73 3.607 (3) 157
Symmetry codes: (i) -x+1, -y+1, -z; (ii) -x+1, -y, -z; (iii) -x+1, -y+1, -z+1; (iv) -x+1, -y, -z+1; (v) x-1, y, z; (vi) -x, -y, -z+1.

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

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536809055275/rz2405sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536809055275/rz2405Isup2.hkl

checkCIF report


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 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, 2009). Herein we report the synthesis and structure of title compound.

The asymmetric unit consists of one molecule of the triangulo-triruthenium complex and one molecule of disordered chloroform solvent (Fig. 1). The bond lengths and angles of title compound are comparable to those found in its related structure (Shawkataly et al., 2009). 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. The phosphine-substituted benzene rings make dihedral angles (C26–C31/C32–C37, C26–C31/C38–C43 and C32–C37/C38–C43) of 68.43 (15), 65.14 (14)and 89.75 (14)° with each other respectively. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 80.70 (15) and 84.53 (16)° for the two diphenylarsino groups respectively.

In the crystal packing (Fig. 2), the molecules are linked into plane parallel to bc plane by intermolecular C10—H10A···O5, C22—H22A···O4, C34—H34A···O4 and C12—H12A···F2 hydrogen bonds. 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 µ-bis(diphenylarsino)methanedecacarbonyltriruthenium(0), see: Bruce et al. (1983). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986).

Experimental top

All manipulations were performed under a dry, oxygen-free dinitrogen atmosphere using standard Schlenk techniques, all solvents were dried over sodium and distilled from sodium benzophenone ketyl under nitrogen. (Pentafluorophenyl)diphenylphosphine (Maybridge) was used as received and µ-bis(diphenylarsino)methane-decacarbonyl-triruthenium(0) (Bruce et al., 1983) were prepared by a reported procedure. The title compound was obtained by refluxing equimolar quantities of Ru3(CO)10(µ-Ph2AsCH2AsPh2) (105.5 mg, 0.1 mmol) and (pentafluorophenyl)diphenylphosphine (35.22 mg, 0.1 mmol) in hexane under nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of C6H14 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 Ueq(C). The chloroform molecule is disordered over two position with the site occupancies are fixed to 0.50 for both components at final refinement. The disordered components were subjected to rigid bond restraint. The minor component was refined isotropically. The maximum and minimum residual electron density peaks of 2.05 and -1.70 e Å-3, respectively, were located 0.44 Å and 0.51 Å from the Cl2B atom.

Structure description 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 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, 2009). Herein we report the synthesis and structure of title compound.

The asymmetric unit consists of one molecule of the triangulo-triruthenium complex and one molecule of disordered chloroform solvent (Fig. 1). The bond lengths and angles of title compound are comparable to those found in its related structure (Shawkataly et al., 2009). 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. The phosphine-substituted benzene rings make dihedral angles (C26–C31/C32–C37, C26–C31/C38–C43 and C32–C37/C38–C43) of 68.43 (15), 65.14 (14)and 89.75 (14)° with each other respectively. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 80.70 (15) and 84.53 (16)° for the two diphenylarsino groups respectively.

In the crystal packing (Fig. 2), the molecules are linked into plane parallel to bc plane by intermolecular C10—H10A···O5, C22—H22A···O4, C34—H34A···O4 and C12—H12A···F2 hydrogen bonds. Weak intermolecular C—H···π interactions further stabilize the crystal structure (Table 1).

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 µ-bis(diphenylarsino)methanedecacarbonyltriruthenium(0), see: Bruce et al. (1983). For the stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986).

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 molecular structure of the title compound with 30% probability ellipsoids for non-H atoms. All disordered components are shown.
[Figure 2] Fig. 2. The crystal packing of the title compound, viewed down the a axis, showing the molecules linked into a plane parallel to bc plane. Hydrogen atoms not involved in the hydrogen-bonding (dashed lines) and the solvent molecules have been omitted for clarity.
[µ-Bis(diphenylarsino)methane-1:2κ2As:As']nonacarbonyl- 1κ3C,2κ3C,3κ3C- [(pentafluorophenyl)diphenylphosphine-3κP]-triangulo- triruthenium(0) chloroform monosolvate top
Crystal data top
[Ru3(C25H22As2)(C18H10F5P)(CO)9]·CHCl3Z = 2
Mr = 1499.16F(000) = 1464
Triclinic, P1Dx = 1.806 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.6354 (3) ÅCell parameters from 9981 reflections
b = 14.1572 (3) Åθ = 2.5–35.0°
c = 16.2418 (4) ŵ = 2.25 mm−1
α = 81.497 (1)°T = 100 K
β = 81.452 (1)°Block, red
γ = 74.994 (1)°0.46 × 0.20 × 0.14 mm
V = 2756.86 (11) Å3
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		15949 independent reflections
Radiation source: fine-focus sealed tube13916 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
φ and ω scansθmax = 30.0°, θmin = 1.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2005)		h = −17→17
Tmin = 0.427, Tmax = 0.745k = −19→19
83481 measured reflectionsl = −22→22
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.088H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0344P)2 + 8.2555P]
where P = (Fo2 + 2Fc2)/3
15949 reflections(Δ/σ)max = 0.001
702 parametersΔρmax = 2.05 e Å−3
6 restraintsΔρmin = −1.70 e Å−3
Crystal data top
[Ru3(C25H22As2)(C18H10F5P)(CO)9]·CHCl3γ = 74.994 (1)°
Mr = 1499.16V = 2756.86 (11) Å3
Triclinic, P1Z = 2
a = 12.6354 (3) ÅMo Kα radiation
b = 14.1572 (3) ŵ = 2.25 mm−1
c = 16.2418 (4) ÅT = 100 K
α = 81.497 (1)°0.46 × 0.20 × 0.14 mm
β = 81.452 (1)°
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer		15949 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2005)		13916 reflections with I > 2σ(I)
Tmin = 0.427, Tmax = 0.745Rint = 0.028
83481 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0326 restraints
wR(F2) = 0.088H-atom parameters constrained
S = 1.07Δρmax = 2.05 e Å−3
15949 reflectionsΔρmin = −1.70 e Å−3
702 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)
Ru10.524202 (17)0.149640 (15)0.235137 (13)0.01477 (5)
Ru20.464067 (17)0.348007 (15)0.276292 (13)0.01422 (5)
Ru30.306485 (17)0.231861 (16)0.312682 (14)0.01602 (5)
As10.69998 (2)0.17494 (2)0.166538 (17)0.01419 (6)
As20.64874 (2)0.37420 (2)0.256950 (17)0.01438 (6)
P10.21075 (6)0.11577 (5)0.29766 (4)0.01570 (13)
F10.32445 (16)0.01111 (13)0.13905 (11)0.0256 (4)
F20.2792 (2)0.06177 (15)−0.01870 (12)0.0350 (5)
F30.10632 (19)0.21441 (16)−0.05752 (12)0.0338 (5)
F4−0.01665 (16)0.32048 (16)0.06474 (13)0.0325 (4)
F50.02756 (14)0.27309 (14)0.22319 (11)0.0247 (4)
O10.41632 (18)0.19539 (17)0.07211 (14)0.0251 (4)
O20.5609 (2)−0.06487 (17)0.20836 (17)0.0336 (5)
O30.61565 (19)0.08889 (18)0.40559 (14)0.0282 (5)
O40.4936 (2)0.28944 (17)0.46205 (14)0.0284 (5)
O50.3194 (2)0.54971 (17)0.30900 (15)0.0319 (5)
O60.45619 (19)0.40229 (17)0.08624 (14)0.0253 (4)
O70.23052 (18)0.35871 (17)0.15241 (15)0.0270 (5)
O80.1254 (2)0.3807 (2)0.40125 (19)0.0401 (6)
O90.3746 (2)0.1271 (2)0.48352 (15)0.0324 (5)
C10.8252 (2)0.0604 (2)0.16541 (18)0.0178 (5)
C20.9180 (2)0.0583 (2)0.10684 (18)0.0196 (5)
H2A0.92020.11140.06600.023*
C31.0078 (2)−0.0238 (2)0.1095 (2)0.0233 (6)
H3A1.0696−0.02510.07020.028*
C41.0053 (3)−0.1031 (2)0.1703 (2)0.0254 (6)
H4A1.0650−0.15770.17190.030*
C50.9128 (3)−0.1009 (2)0.2292 (2)0.0268 (6)
H5A0.9112−0.15370.27040.032*
C60.8228 (2)−0.0199 (2)0.22656 (19)0.0216 (5)
H6A0.7608−0.01910.26560.026*
C70.7080 (2)0.2292 (2)0.04967 (16)0.0168 (5)
C80.7381 (3)0.3180 (2)0.02187 (19)0.0232 (6)
H8A0.75720.35250.05950.028*
C90.7392 (3)0.3543 (2)−0.0628 (2)0.0289 (7)
H9A0.75870.4135−0.08150.035*
C100.7116 (3)0.3027 (2)−0.11942 (19)0.0281 (7)
H10A0.71320.3270−0.17590.034*
C110.6815 (3)0.2148 (2)−0.09154 (19)0.0259 (6)
H11A0.66320.1801−0.12950.031*
C120.6786 (2)0.1783 (2)−0.00691 (18)0.0211 (5)
H12A0.65720.12000.01170.025*
C130.7620 (2)0.2601 (2)0.22097 (17)0.0162 (5)
H13A0.79590.22240.26930.019*
H13B0.81900.28250.18220.019*
C140.6792 (2)0.4828 (2)0.17732 (17)0.0175 (5)
C150.5925 (2)0.5543 (2)0.14568 (18)0.0212 (5)
H15A0.52020.55060.16370.025*
C160.6136 (3)0.6314 (2)0.0871 (2)0.0256 (6)
H16A0.55550.67920.06590.031*
C170.7214 (3)0.6368 (3)0.0605 (2)0.0289 (7)
H17A0.73560.68770.02070.035*
C180.8085 (3)0.5662 (3)0.0930 (2)0.0277 (6)
H18A0.88080.57010.07500.033*
C190.7876 (2)0.4900 (2)0.1523 (2)0.0222 (6)
H19A0.84560.44380.17530.027*
C200.7044 (2)0.4011 (2)0.35381 (17)0.0181 (5)
C210.6342 (3)0.4680 (3)0.4041 (2)0.0320 (7)
H21A0.56210.49570.39210.038*
C220.6710 (3)0.4935 (3)0.4722 (3)0.0400 (9)
H22A0.62350.53800.50590.048*
C230.7785 (3)0.4529 (3)0.4900 (2)0.0295 (7)
H23A0.80320.47070.53520.035*
C240.8481 (3)0.3866 (2)0.4410 (2)0.0257 (6)
H24A0.92010.35930.45320.031*
C250.8117 (2)0.3596 (2)0.37293 (19)0.0219 (5)
H25A0.85910.31390.34030.026*
C260.1728 (2)0.1353 (2)0.19005 (17)0.0180 (5)
C270.2360 (2)0.0849 (2)0.12485 (18)0.0205 (5)
C280.2146 (3)0.1108 (2)0.04191 (18)0.0244 (6)
C290.1278 (3)0.1885 (2)0.02168 (19)0.0257 (6)
C300.0648 (2)0.2423 (2)0.08410 (19)0.0234 (6)
C310.0880 (2)0.2150 (2)0.16600 (18)0.0199 (5)
C320.2689 (2)−0.0174 (2)0.31666 (17)0.0187 (5)
C330.3620 (3)−0.0532 (2)0.35865 (19)0.0238 (6)
H33A0.3986−0.00950.37230.029*
C340.4008 (3)−0.1537 (3)0.3805 (2)0.0303 (7)
H34A0.4637−0.17680.40790.036*
C350.3467 (3)−0.2193 (2)0.3617 (2)0.0305 (7)
H35A0.3723−0.28650.37710.037*
C360.2530 (3)−0.1846 (2)0.3193 (2)0.0269 (6)
H36A0.2164−0.22870.30640.032*
C370.2147 (3)−0.0846 (2)0.29670 (18)0.0223 (6)
H37A0.1527−0.06190.26810.027*
C380.0781 (2)0.1203 (2)0.36324 (17)0.0179 (5)
C39−0.0093 (2)0.0919 (2)0.33857 (18)0.0196 (5)
H39A−0.00490.07620.28440.023*
C40−0.1028 (2)0.0870 (2)0.39465 (19)0.0213 (5)
H40A−0.16040.06760.37780.026*
C41−0.1109 (2)0.1109 (2)0.4755 (2)0.0241 (6)
H41A−0.17400.10840.51240.029*
C42−0.0244 (3)0.1386 (2)0.50100 (18)0.0233 (6)
H42A−0.02900.15370.55540.028*
C430.0695 (2)0.1438 (2)0.44474 (18)0.0206 (5)
H43A0.12690.16310.46180.025*
C440.4530 (2)0.1837 (2)0.13446 (18)0.0194 (5)
C450.5443 (2)0.0156 (2)0.21989 (19)0.0225 (6)
C460.5774 (2)0.1157 (2)0.34376 (18)0.0201 (5)
C470.4802 (2)0.3059 (2)0.39310 (19)0.0205 (5)
C480.3746 (2)0.4735 (2)0.29795 (17)0.0201 (5)
C490.4575 (2)0.3773 (2)0.15634 (18)0.0190 (5)
C500.2671 (2)0.3107 (2)0.20913 (19)0.0216 (5)
C510.1929 (3)0.3231 (2)0.3690 (2)0.0253 (6)
C520.3560 (2)0.1641 (2)0.41851 (19)0.0225 (6)
Cl1A0.9948 (5)0.6545 (2)0.3796 (2)0.1120 (18)0.50
Cl2A0.8101 (3)0.6591 (3)0.2961 (3)0.0877 (11)0.50
Cl3A1.0299 (3)0.5688 (6)0.2281 (2)0.128 (2)0.50
C53A0.9402 (11)0.5940 (8)0.3180 (6)0.071 (4)0.50
H53A0.93340.53100.34970.086*0.50
Cl1B0.7461 (4)0.7106 (3)0.2760 (3)0.0970 (12)*0.50
Cl2B0.8857 (6)0.6721 (5)0.4055 (4)0.140 (2)*0.50
Cl3B0.9765 (4)0.6119 (4)0.2435 (3)0.1025 (13)*0.50
C53B0.8682 (13)0.6310 (13)0.3144 (10)0.089 (5)*0.50
H53B0.85120.56670.33160.107*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01463 (9)0.01510 (9)0.01545 (10)−0.00625 (7)−0.00122 (7)−0.00026 (7)
Ru20.01310 (9)0.01471 (9)0.01522 (9)−0.00497 (7)−0.00170 (7)0.00006 (7)
Ru30.01377 (9)0.01956 (10)0.01610 (10)−0.00761 (8)−0.00084 (7)−0.00084 (8)
As10.01427 (12)0.01494 (12)0.01388 (12)−0.00502 (9)−0.00136 (9)−0.00087 (9)
As20.01357 (12)0.01500 (12)0.01544 (12)−0.00520 (9)−0.00202 (9)−0.00102 (9)
P10.0148 (3)0.0191 (3)0.0140 (3)−0.0069 (2)−0.0010 (2)−0.0003 (2)
F10.0305 (9)0.0228 (9)0.0207 (8)−0.0047 (7)0.0020 (7)−0.0019 (7)
F20.0597 (14)0.0280 (10)0.0167 (9)−0.0118 (9)0.0032 (9)−0.0057 (7)
F30.0493 (12)0.0416 (11)0.0174 (9)−0.0225 (10)−0.0128 (8)0.0045 (8)
F40.0237 (9)0.0416 (11)0.0290 (10)−0.0067 (8)−0.0095 (8)0.0106 (8)
F50.0184 (8)0.0305 (9)0.0216 (8)−0.0033 (7)0.0003 (6)0.0010 (7)
O10.0257 (11)0.0286 (11)0.0233 (10)−0.0106 (9)−0.0079 (8)0.0014 (9)
O20.0416 (14)0.0218 (11)0.0388 (14)−0.0118 (10)0.0015 (11)−0.0069 (10)
O30.0284 (11)0.0310 (12)0.0222 (11)−0.0029 (9)−0.0054 (9)0.0007 (9)
O40.0379 (13)0.0264 (11)0.0218 (11)−0.0098 (10)−0.0083 (9)0.0030 (9)
O50.0406 (14)0.0228 (11)0.0251 (11)0.0018 (10)0.0015 (10)−0.0018 (9)
O60.0290 (11)0.0296 (11)0.0200 (10)−0.0128 (9)−0.0051 (8)0.0012 (8)
O70.0228 (11)0.0312 (12)0.0276 (11)−0.0112 (9)−0.0065 (9)0.0065 (9)
O80.0289 (13)0.0386 (14)0.0540 (17)−0.0081 (11)0.0100 (12)−0.0237 (13)
O90.0336 (13)0.0451 (14)0.0220 (11)−0.0191 (11)−0.0063 (9)0.0057 (10)
C10.0175 (12)0.0177 (12)0.0193 (12)−0.0049 (10)−0.0032 (10)−0.0037 (10)
C20.0196 (13)0.0227 (13)0.0186 (12)−0.0077 (10)−0.0007 (10)−0.0062 (10)
C30.0178 (13)0.0263 (14)0.0277 (15)−0.0050 (11)−0.0011 (11)−0.0113 (12)
C40.0218 (14)0.0222 (14)0.0323 (16)0.0001 (11)−0.0083 (12)−0.0083 (12)
C50.0284 (15)0.0204 (14)0.0304 (16)−0.0036 (12)−0.0077 (12)0.0010 (12)
C60.0211 (13)0.0208 (13)0.0224 (13)−0.0051 (11)−0.0035 (10)−0.0001 (11)
C70.0176 (12)0.0178 (12)0.0138 (11)−0.0028 (10)−0.0014 (9)−0.0010 (9)
C80.0288 (15)0.0218 (13)0.0199 (13)−0.0094 (11)−0.0014 (11)−0.0015 (11)
C90.0380 (18)0.0224 (14)0.0232 (15)−0.0074 (13)0.0009 (13)0.0027 (11)
C100.0335 (17)0.0284 (15)0.0158 (13)0.0016 (13)−0.0024 (11)0.0015 (11)
C110.0290 (15)0.0291 (15)0.0192 (13)−0.0032 (12)−0.0050 (11)−0.0057 (11)
C120.0232 (13)0.0204 (13)0.0196 (13)−0.0049 (11)−0.0032 (10)−0.0023 (10)
C130.0148 (11)0.0172 (12)0.0171 (12)−0.0043 (9)−0.0025 (9)−0.0026 (9)
C140.0203 (13)0.0178 (12)0.0158 (12)−0.0074 (10)−0.0022 (10)−0.0010 (9)
C150.0191 (13)0.0246 (14)0.0212 (13)−0.0077 (11)−0.0041 (10)−0.0009 (11)
C160.0277 (15)0.0254 (14)0.0253 (15)−0.0119 (12)−0.0086 (12)0.0075 (12)
C170.0324 (16)0.0299 (16)0.0278 (15)−0.0185 (13)−0.0071 (13)0.0089 (12)
C180.0234 (14)0.0317 (16)0.0310 (16)−0.0161 (13)−0.0037 (12)0.0039 (13)
C190.0196 (13)0.0216 (13)0.0277 (14)−0.0096 (11)−0.0042 (11)0.0001 (11)
C200.0185 (12)0.0190 (12)0.0183 (12)−0.0067 (10)−0.0025 (10)−0.0032 (10)
C210.0228 (15)0.0383 (18)0.0352 (18)0.0006 (13)−0.0047 (13)−0.0181 (15)
C220.0331 (18)0.050 (2)0.040 (2)−0.0014 (16)−0.0035 (15)−0.0302 (18)
C230.0327 (17)0.0384 (18)0.0231 (15)−0.0135 (14)−0.0041 (12)−0.0118 (13)
C240.0234 (14)0.0300 (15)0.0269 (15)−0.0082 (12)−0.0078 (12)−0.0053 (12)
C250.0196 (13)0.0240 (14)0.0235 (14)−0.0046 (11)−0.0038 (10)−0.0066 (11)
C260.0182 (12)0.0239 (13)0.0146 (11)−0.0116 (10)−0.0012 (9)−0.0003 (10)
C270.0245 (14)0.0209 (13)0.0181 (12)−0.0112 (11)−0.0005 (10)−0.0006 (10)
C280.0360 (16)0.0250 (14)0.0163 (13)−0.0166 (13)0.0000 (11)−0.0021 (11)
C290.0337 (16)0.0307 (15)0.0195 (13)−0.0208 (13)−0.0078 (12)0.0029 (11)
C300.0183 (13)0.0292 (15)0.0244 (14)−0.0122 (11)−0.0065 (11)0.0071 (11)
C310.0172 (12)0.0258 (14)0.0179 (12)−0.0105 (11)0.0000 (10)0.0010 (10)
C320.0205 (13)0.0201 (12)0.0158 (12)−0.0078 (10)0.0005 (10)−0.0003 (10)
C330.0249 (14)0.0248 (14)0.0222 (14)−0.0082 (11)−0.0046 (11)0.0016 (11)
C340.0318 (16)0.0291 (16)0.0267 (16)−0.0065 (13)−0.0073 (13)0.0093 (13)
C350.0404 (19)0.0198 (14)0.0276 (16)−0.0057 (13)−0.0023 (13)0.0043 (12)
C360.0374 (17)0.0229 (14)0.0217 (14)−0.0123 (13)0.0018 (12)−0.0033 (11)
C370.0258 (14)0.0239 (14)0.0193 (13)−0.0093 (11)−0.0010 (11)−0.0044 (11)
C380.0167 (12)0.0208 (12)0.0160 (12)−0.0070 (10)0.0002 (9)0.0008 (10)
C390.0183 (12)0.0211 (13)0.0195 (13)−0.0070 (10)−0.0025 (10)0.0012 (10)
C400.0154 (12)0.0251 (14)0.0235 (14)−0.0087 (10)−0.0016 (10)0.0032 (11)
C410.0199 (13)0.0250 (14)0.0249 (14)−0.0071 (11)0.0038 (11)0.0013 (11)
C420.0262 (14)0.0265 (14)0.0167 (13)−0.0086 (12)0.0025 (11)−0.0021 (11)
C430.0205 (13)0.0239 (13)0.0191 (13)−0.0095 (11)−0.0015 (10)−0.0012 (10)
C440.0191 (12)0.0180 (12)0.0223 (13)−0.0084 (10)−0.0012 (10)−0.0005 (10)
C450.0225 (13)0.0242 (14)0.0217 (13)−0.0096 (11)−0.0007 (11)0.0002 (11)
C460.0180 (12)0.0195 (12)0.0214 (13)−0.0045 (10)0.0010 (10)−0.0014 (10)
C470.0208 (13)0.0176 (12)0.0227 (13)−0.0056 (10)−0.0018 (10)0.0002 (10)
C480.0219 (13)0.0213 (13)0.0159 (12)−0.0060 (11)−0.0003 (10)0.0010 (10)
C490.0168 (12)0.0210 (13)0.0212 (13)−0.0086 (10)−0.0016 (10)−0.0020 (10)
C500.0173 (12)0.0238 (14)0.0252 (14)−0.0100 (11)−0.0010 (10)0.0000 (11)
C510.0224 (14)0.0276 (15)0.0280 (15)−0.0112 (12)0.0013 (11)−0.0048 (12)
C520.0202 (13)0.0279 (14)0.0225 (14)−0.0120 (11)−0.0011 (10)−0.0027 (11)
Cl1A0.209 (5)0.0446 (14)0.092 (2)0.009 (2)−0.112 (3)−0.0128 (14)
Cl2A0.068 (2)0.097 (3)0.120 (3)−0.049 (2)0.006 (2)−0.047 (2)
Cl3A0.060 (2)0.275 (7)0.0578 (19)−0.041 (3)0.0028 (15)−0.055 (3)
C53A0.116 (11)0.045 (5)0.055 (6)−0.042 (7)0.034 (7)−0.015 (5)
Geometric parameters (Å, º) top
Ru1—C451.897 (3)C13—H13A0.9700
Ru1—C441.922 (3)C13—H13B0.9700
Ru1—C461.931 (3)C14—C151.388 (4)
Ru1—As12.4210 (3)C14—C191.395 (4)
Ru1—Ru22.8653 (3)C15—C161.392 (4)
Ru1—Ru32.8730 (3)C15—H15A0.9300
Ru2—C481.894 (3)C16—C171.384 (5)
Ru2—C471.927 (3)C16—H16A0.9300
Ru2—C491.940 (3)C17—C181.391 (5)
Ru2—As22.4243 (3)C17—H17A0.9300
Ru2—Ru32.8418 (3)C18—C191.389 (4)
Ru3—C511.887 (3)C18—H18A0.9300
Ru3—C501.931 (3)C19—H19A0.9300
Ru3—C521.946 (3)C20—C211.389 (4)
Ru3—P12.3367 (7)C20—C251.392 (4)
As1—C71.938 (3)C21—C221.390 (5)
As1—C11.951 (3)C21—H21A0.9300
As1—C131.964 (3)C22—C231.385 (5)
As2—C141.937 (3)C22—H22A0.9300
As2—C201.939 (3)C23—C241.369 (5)
As2—C131.958 (3)C23—H23A0.9300
P1—C321.835 (3)C24—C251.396 (4)
P1—C381.839 (3)C24—H24A0.9300
P1—C261.844 (3)C25—H25A0.9300
F1—C271.339 (3)C26—C311.393 (4)
F2—C281.337 (4)C26—C271.395 (4)
F3—C291.333 (3)C27—C281.390 (4)
F4—C301.337 (4)C28—C291.377 (5)
F5—C311.346 (3)C29—C301.384 (5)
O1—C441.148 (4)C30—C311.382 (4)
O2—C451.142 (4)C32—C331.390 (4)
O3—C461.150 (4)C32—C371.405 (4)
O4—C471.139 (4)C33—C341.390 (4)
O5—C481.146 (4)C33—H33A0.9300
O6—C491.143 (4)C34—C351.378 (5)
O7—C501.142 (4)C34—H34A0.9300
O8—C511.140 (4)C35—C361.399 (5)
O9—C521.136 (4)C35—H35A0.9300
C1—C21.392 (4)C36—C371.385 (4)
C1—C61.398 (4)C36—H36A0.9300
C2—C31.399 (4)C37—H37A0.9300
C2—H2A0.9300C38—C431.394 (4)
C3—C41.386 (5)C38—C391.396 (4)
C3—H3A0.9300C39—C401.391 (4)
C4—C51.392 (5)C39—H39A0.9300
C4—H4A0.9300C40—C411.386 (4)
C5—C61.391 (4)C40—H40A0.9300
C5—H5A0.9300C41—C421.387 (4)
C6—H6A0.9300C41—H41A0.9300
C7—C121.392 (4)C42—C431.396 (4)
C7—C81.398 (4)C42—H42A0.9300
C8—C91.395 (4)C43—H43A0.9300
C8—H8A0.9300Cl1A—C53A1.725 (11)
C9—C101.388 (5)Cl2A—C53A1.723 (14)
C9—H9A0.9300Cl3A—C53A1.731 (10)
C10—C111.388 (5)C53A—H53A0.9800
C10—H10A0.9300Cl1B—C53B1.794 (14)
C11—C121.394 (4)Cl2B—C53B1.731 (16)
C11—H11A0.9300Cl3B—C53B1.644 (15)
C12—H12A0.9300C53B—H53B0.9800
C45—Ru1—C4487.69 (13)C14—C15—C16120.2 (3)
C45—Ru1—C4692.37 (13)C14—C15—H15A119.9
C44—Ru1—C46172.77 (12)C16—C15—H15A119.9
C45—Ru1—As199.18 (9)C17—C16—C15119.8 (3)
C44—Ru1—As194.51 (8)C17—C16—H16A120.1
C46—Ru1—As192.62 (8)C15—C16—H16A120.1
C45—Ru1—Ru2170.93 (9)C16—C17—C18120.3 (3)
C44—Ru1—Ru293.53 (9)C16—C17—H17A119.9
C46—Ru1—Ru285.29 (9)C18—C17—H17A119.9
As1—Ru1—Ru289.691 (10)C19—C18—C17120.0 (3)
C45—Ru1—Ru3111.96 (9)C19—C18—H18A120.0
C44—Ru1—Ru383.03 (9)C17—C18—H18A120.0
C46—Ru1—Ru390.25 (8)C18—C19—C14119.8 (3)
As1—Ru1—Ru3148.582 (12)C18—C19—H19A120.1
Ru2—Ru1—Ru359.370 (7)C14—C19—H19A120.1
C48—Ru2—C4793.06 (12)C21—C20—C25119.2 (3)
C48—Ru2—C4992.85 (12)C21—C20—As2117.6 (2)
C47—Ru2—C49174.09 (12)C25—C20—As2123.1 (2)
C48—Ru2—As2102.74 (9)C20—C21—C22120.2 (3)
C47—Ru2—As288.81 (9)C20—C21—H21A119.9
C49—Ru2—As289.79 (8)C22—C21—H21A119.9
C48—Ru2—Ru3101.06 (9)C23—C22—C21120.1 (3)
C47—Ru2—Ru380.96 (9)C23—C22—H22A119.9
C49—Ru2—Ru398.00 (8)C21—C22—H22A119.9
As2—Ru2—Ru3154.528 (12)C24—C23—C22120.0 (3)
C48—Ru2—Ru1159.52 (9)C24—C23—H23A120.0
C47—Ru2—Ru192.48 (9)C22—C23—H23A120.0
C49—Ru2—Ru182.00 (9)C23—C24—C25120.4 (3)
As2—Ru2—Ru197.077 (10)C23—C24—H24A119.8
Ru3—Ru2—Ru160.450 (7)C25—C24—H24A119.8
C51—Ru3—C5087.52 (14)C20—C25—C24120.0 (3)
C51—Ru3—C5291.29 (14)C20—C25—H25A120.0
C50—Ru3—C52173.07 (12)C24—C25—H25A120.0
C51—Ru3—P1100.25 (9)C31—C26—C27115.3 (3)
C50—Ru3—P193.42 (9)C31—C26—P1120.1 (2)
C52—Ru3—P193.52 (9)C27—C26—P1123.6 (2)
C51—Ru3—Ru297.64 (9)F1—C27—C28116.5 (3)
C50—Ru3—Ru276.95 (8)F1—C27—C26121.0 (3)
C52—Ru3—Ru296.46 (8)C28—C27—C26122.5 (3)
P1—Ru3—Ru2159.28 (2)F2—C28—C29119.7 (3)
C51—Ru3—Ru1157.38 (9)F2—C28—C27120.3 (3)
C50—Ru3—Ru191.23 (9)C29—C28—C27120.0 (3)
C52—Ru3—Ru187.24 (9)F3—C29—C28120.7 (3)
P1—Ru3—Ru1102.374 (19)F3—C29—C30119.8 (3)
Ru2—Ru3—Ru160.180 (7)C28—C29—C30119.4 (3)
C7—As1—C1101.81 (11)F4—C30—C31120.7 (3)
C7—As1—C13104.16 (11)F4—C30—C29120.0 (3)
C1—As1—C1398.63 (11)C31—C30—C29119.3 (3)
C7—As1—Ru1117.89 (8)F5—C31—C30116.5 (3)
C1—As1—Ru1117.30 (8)F5—C31—C26119.9 (2)
C13—As1—Ru1114.39 (8)C30—C31—C26123.4 (3)
C14—As2—C2099.53 (12)C33—C32—C37118.8 (3)
C14—As2—C13103.74 (12)C33—C32—P1119.9 (2)
C20—As2—C13102.41 (11)C37—C32—P1120.9 (2)
C14—As2—Ru2118.35 (8)C34—C33—C32120.6 (3)
C20—As2—Ru2117.46 (8)C34—C33—H33A119.7
C13—As2—Ru2113.05 (8)C32—C33—H33A119.7
C32—P1—C3897.60 (13)C35—C34—C33120.4 (3)
C32—P1—C26104.34 (13)C35—C34—H34A119.8
C38—P1—C26103.31 (13)C33—C34—H34A119.8
C32—P1—Ru3122.83 (10)C34—C35—C36119.8 (3)
C38—P1—Ru3117.20 (10)C34—C35—H35A120.1
C26—P1—Ru3109.21 (9)C36—C35—H35A120.1
C2—C1—C6119.5 (3)C37—C36—C35120.0 (3)
C2—C1—As1121.4 (2)C37—C36—H36A120.0
C6—C1—As1119.0 (2)C35—C36—H36A120.0
C1—C2—C3120.0 (3)C36—C37—C32120.4 (3)
C1—C2—H2A120.0C36—C37—H37A119.8
C3—C2—H2A120.0C32—C37—H37A119.8
C4—C3—C2120.4 (3)C43—C38—C39118.8 (3)
C4—C3—H3A119.8C43—C38—P1117.6 (2)
C2—C3—H3A119.8C39—C38—P1123.4 (2)
C3—C4—C5119.7 (3)C40—C39—C38120.4 (3)
C3—C4—H4A120.2C40—C39—H39A119.8
C5—C4—H4A120.2C38—C39—H39A119.8
C6—C5—C4120.3 (3)C41—C40—C39120.5 (3)
C6—C5—H5A119.8C41—C40—H40A119.8
C4—C5—H5A119.8C39—C40—H40A119.8
C5—C6—C1120.2 (3)C40—C41—C42119.8 (3)
C5—C6—H6A119.9C40—C41—H41A120.1
C1—C6—H6A119.9C42—C41—H41A120.1
C12—C7—C8120.0 (3)C41—C42—C43119.8 (3)
C12—C7—As1117.6 (2)C41—C42—H42A120.1
C8—C7—As1122.4 (2)C43—C42—H42A120.1
C9—C8—C7119.5 (3)C38—C43—C42120.8 (3)
C9—C8—H8A120.3C38—C43—H43A119.6
C7—C8—H8A120.3C42—C43—H43A119.6
C10—C9—C8120.5 (3)O1—C44—Ru1173.4 (3)
C10—C9—H9A119.8O2—C45—Ru1176.8 (3)
C8—C9—H9A119.8O3—C46—Ru1174.1 (3)
C11—C10—C9119.9 (3)O4—C47—Ru2172.9 (3)
C11—C10—H10A120.1O5—C48—Ru2178.1 (3)
C9—C10—H10A120.1O6—C49—Ru2173.8 (3)
C10—C11—C12120.2 (3)O7—C50—Ru3171.5 (3)
C10—C11—H11A119.9O8—C51—Ru3177.7 (3)
C12—C11—H11A119.9O9—C52—Ru3173.4 (3)
C7—C12—C11120.0 (3)Cl2A—C53A—Cl1A111.5 (6)
C7—C12—H12A120.0Cl2A—C53A—Cl3A112.4 (7)
C11—C12—H12A120.0Cl1A—C53A—Cl3A109.9 (7)
As2—C13—As1111.64 (13)Cl2A—C53A—H53A107.6
As2—C13—H13A109.3Cl1A—C53A—H53A107.6
As1—C13—H13A109.3Cl3A—C53A—H53A107.6
As2—C13—H13B109.3Cl3B—C53B—Cl2B116.4 (10)
As1—C13—H13B109.3Cl3B—C53B—Cl1B114.4 (9)
H13A—C13—H13B108.0Cl2B—C53B—Cl1B107.6 (9)
C15—C14—C19119.9 (3)Cl3B—C53B—H53B105.9
C15—C14—As2119.8 (2)Cl2B—C53B—H53B105.9
C19—C14—As2120.3 (2)Cl1B—C53B—H53B105.9
C44—Ru1—Ru2—C4852.3 (3)C13—As1—C1—C6100.1 (2)
C46—Ru1—Ru2—C48−120.5 (3)Ru1—As1—C1—C6−23.2 (3)
As1—Ru1—Ru2—C48146.8 (2)C6—C1—C2—C30.0 (4)
Ru3—Ru1—Ru2—C48−27.4 (2)As1—C1—C2—C3177.9 (2)
C44—Ru1—Ru2—C47157.91 (12)C1—C2—C3—C4−0.2 (4)
C46—Ru1—Ru2—C47−14.94 (12)C2—C3—C4—C5−0.1 (5)
As1—Ru1—Ru2—C47−107.60 (9)C3—C4—C5—C60.6 (5)
Ru3—Ru1—Ru2—C4778.15 (9)C4—C5—C6—C1−0.8 (5)
C44—Ru1—Ru2—C49−24.20 (12)C2—C1—C6—C50.5 (4)
C46—Ru1—Ru2—C49162.95 (12)As1—C1—C6—C5−177.5 (2)
As1—Ru1—Ru2—C4970.29 (8)C1—As1—C7—C1272.1 (2)
Ru3—Ru1—Ru2—C49−103.96 (8)C13—As1—C7—C12174.2 (2)
C44—Ru1—Ru2—As2−112.99 (8)Ru1—As1—C7—C12−57.8 (2)
C46—Ru1—Ru2—As274.16 (8)C1—As1—C7—C8−110.1 (2)
As1—Ru1—Ru2—As2−18.492 (12)C13—As1—C7—C8−7.9 (3)
Ru3—Ru1—Ru2—As2167.256 (12)Ru1—As1—C7—C8120.0 (2)
C44—Ru1—Ru2—Ru379.75 (8)C12—C7—C8—C9−0.5 (5)
C46—Ru1—Ru2—Ru3−93.09 (8)As1—C7—C8—C9−178.2 (2)
As1—Ru1—Ru2—Ru3174.251 (11)C7—C8—C9—C10−0.5 (5)
C48—Ru2—Ru3—C51−14.21 (13)C8—C9—C10—C110.6 (5)
C47—Ru2—Ru3—C5177.17 (14)C9—C10—C11—C120.2 (5)
C49—Ru2—Ru3—C51−108.71 (13)C8—C7—C12—C111.3 (4)
As2—Ru2—Ru3—C51144.65 (11)As1—C7—C12—C11179.2 (2)
Ru1—Ru2—Ru3—C51175.25 (10)C10—C11—C12—C7−1.2 (5)
C48—Ru2—Ru3—C5071.44 (13)C14—As2—C13—As1−106.55 (14)
C47—Ru2—Ru3—C50162.82 (13)C20—As2—C13—As1150.25 (13)
C49—Ru2—Ru3—C50−23.07 (13)Ru2—As2—C13—As122.89 (15)
As2—Ru2—Ru3—C50−129.70 (10)C7—As1—C13—As288.09 (14)
Ru1—Ru2—Ru3—C50−99.10 (9)C1—As1—C13—As2−167.33 (13)
C48—Ru2—Ru3—C52−106.39 (13)Ru1—As1—C13—As2−42.01 (15)
C47—Ru2—Ru3—C52−15.01 (13)C20—As2—C14—C15−115.7 (2)
C49—Ru2—Ru3—C52159.11 (13)C13—As2—C14—C15138.9 (2)
As2—Ru2—Ru3—C5252.47 (10)Ru2—As2—C14—C1512.8 (3)
Ru1—Ru2—Ru3—C5283.07 (9)C20—As2—C14—C1963.6 (3)
C48—Ru2—Ru3—P1135.34 (10)C13—As2—C14—C19−41.8 (3)
C47—Ru2—Ru3—P1−133.28 (10)Ru2—As2—C14—C19−167.9 (2)
C49—Ru2—Ru3—P140.83 (10)C19—C14—C15—C162.0 (4)
As2—Ru2—Ru3—P1−65.80 (7)As2—C14—C15—C16−178.6 (2)
Ru1—Ru2—Ru3—P1−35.20 (6)C14—C15—C16—C17−0.1 (5)
C48—Ru2—Ru3—Ru1170.54 (9)C15—C16—C17—C18−1.0 (5)
C47—Ru2—Ru3—Ru1−98.08 (9)C16—C17—C18—C190.1 (5)
C49—Ru2—Ru3—Ru176.04 (9)C17—C18—C19—C141.9 (5)
As2—Ru2—Ru3—Ru1−30.60 (3)C15—C14—C19—C18−2.9 (5)
C45—Ru1—Ru3—C51164.7 (3)As2—C14—C19—C18177.7 (2)
C44—Ru1—Ru3—C51−110.6 (3)C14—As2—C20—C2184.5 (3)
C46—Ru1—Ru3—C5172.0 (3)C13—As2—C20—C21−169.1 (3)
As1—Ru1—Ru3—C51−23.4 (3)Ru2—As2—C20—C21−44.6 (3)
Ru2—Ru1—Ru3—C51−12.3 (3)C14—As2—C20—C25−93.0 (3)
C45—Ru1—Ru3—C50−108.79 (13)C13—As2—C20—C2513.4 (3)
C44—Ru1—Ru3—C50−24.13 (12)Ru2—As2—C20—C25137.9 (2)
C46—Ru1—Ru3—C50158.55 (12)C25—C20—C21—C220.5 (5)
As1—Ru1—Ru3—C5063.10 (9)As2—C20—C21—C22−177.1 (3)
Ru2—Ru1—Ru3—C5074.18 (9)C20—C21—C22—C230.4 (6)
C45—Ru1—Ru3—C5277.98 (13)C21—C22—C23—C24−0.7 (6)
C44—Ru1—Ru3—C52162.64 (12)C22—C23—C24—C250.1 (5)
C46—Ru1—Ru3—C52−14.68 (12)C21—C20—C25—C24−1.1 (5)
As1—Ru1—Ru3—C52−110.13 (9)As2—C20—C25—C24176.4 (2)
Ru2—Ru1—Ru3—C52−99.05 (9)C23—C24—C25—C200.8 (5)
C45—Ru1—Ru3—P1−15.02 (10)C32—P1—C26—C31153.1 (2)
C44—Ru1—Ru3—P169.64 (8)C38—P1—C26—C3151.5 (2)
C46—Ru1—Ru3—P1−107.68 (9)Ru3—P1—C26—C31−73.9 (2)
As1—Ru1—Ru3—P1156.87 (3)C32—P1—C26—C27−38.5 (3)
Ru2—Ru1—Ru3—P1167.95 (2)C38—P1—C26—C27−140.1 (2)
C45—Ru1—Ru3—Ru2177.03 (10)Ru3—P1—C26—C2794.4 (2)
C44—Ru1—Ru3—Ru2−98.31 (8)C31—C26—C27—F1175.4 (2)
C46—Ru1—Ru3—Ru284.37 (9)P1—C26—C27—F16.6 (4)
As1—Ru1—Ru3—Ru2−11.08 (2)C31—C26—C27—C28−1.4 (4)
C45—Ru1—As1—C794.63 (13)P1—C26—C27—C28−170.2 (2)
C44—Ru1—As1—C76.24 (13)F1—C27—C28—F21.4 (4)
C46—Ru1—As1—C7−172.54 (13)C26—C27—C28—F2178.4 (3)
Ru2—Ru1—As1—C7−87.27 (9)F1—C27—C28—C29−177.4 (3)
Ru3—Ru1—As1—C7−77.76 (10)C26—C27—C28—C29−0.4 (4)
C45—Ru1—As1—C1−27.62 (13)F2—C28—C29—F31.0 (4)
C44—Ru1—As1—C1−116.01 (13)C27—C28—C29—F3179.9 (3)
C46—Ru1—As1—C165.21 (13)F2—C28—C29—C30−176.6 (3)
Ru2—Ru1—As1—C1150.47 (9)C27—C28—C29—C302.3 (4)
Ru3—Ru1—As1—C1159.99 (9)F3—C29—C30—F4−0.5 (4)
C45—Ru1—As1—C13−142.42 (13)C28—C29—C30—F4177.1 (3)
C44—Ru1—As1—C13129.19 (12)F3—C29—C30—C31−179.8 (3)
C46—Ru1—As1—C13−49.59 (12)C28—C29—C30—C31−2.1 (4)
Ru2—Ru1—As1—C1335.68 (9)F4—C30—C31—F5−2.5 (4)
Ru3—Ru1—As1—C1345.19 (9)C29—C30—C31—F5176.8 (3)
C48—Ru2—As2—C14−52.19 (13)F4—C30—C31—C26−179.0 (3)
C47—Ru2—As2—C14−145.06 (13)C29—C30—C31—C260.2 (4)
C49—Ru2—As2—C1440.68 (13)C27—C26—C31—F5−174.9 (2)
Ru3—Ru2—As2—C14149.09 (10)P1—C26—C31—F5−5.7 (4)
Ru1—Ru2—As2—C14122.59 (9)C27—C26—C31—C301.5 (4)
C48—Ru2—As2—C2067.30 (13)P1—C26—C31—C30170.8 (2)
C47—Ru2—As2—C20−25.57 (13)C38—P1—C32—C33−114.9 (2)
C49—Ru2—As2—C20160.18 (13)C26—P1—C32—C33139.2 (2)
Ru3—Ru2—As2—C20−91.42 (10)Ru3—P1—C32—C3314.5 (3)
Ru1—Ru2—As2—C20−117.92 (9)C38—P1—C32—C3758.8 (3)
C48—Ru2—As2—C13−173.72 (12)C26—P1—C32—C37−47.1 (3)
C47—Ru2—As2—C1393.41 (12)Ru3—P1—C32—C37−171.80 (19)
C49—Ru2—As2—C13−80.85 (12)C37—C32—C33—C340.0 (4)
Ru3—Ru2—As2—C1327.56 (9)P1—C32—C33—C34173.9 (2)
Ru1—Ru2—As2—C131.06 (9)C32—C33—C34—C35−0.8 (5)
C51—Ru3—P1—C32−136.81 (15)C33—C34—C35—C360.9 (5)
C50—Ru3—P1—C32135.09 (14)C34—C35—C36—C37−0.2 (5)
C52—Ru3—P1—C32−44.86 (14)C35—C36—C37—C32−0.5 (5)
Ru2—Ru3—P1—C3273.88 (12)C33—C32—C37—C360.6 (4)
Ru1—Ru3—P1—C3243.08 (11)P1—C32—C37—C36−173.2 (2)
C51—Ru3—P1—C38−16.24 (14)C32—P1—C38—C4396.1 (2)
C50—Ru3—P1—C38−104.34 (14)C26—P1—C38—C43−157.1 (2)
C52—Ru3—P1—C3875.70 (14)Ru3—P1—C38—C43−37.0 (3)
Ru2—Ru3—P1—C38−165.55 (10)C32—P1—C38—C39−77.2 (3)
Ru1—Ru3—P1—C38163.65 (10)C26—P1—C38—C3929.6 (3)
C51—Ru3—P1—C26100.71 (14)Ru3—P1—C38—C39149.7 (2)
C50—Ru3—P1—C2612.61 (13)C43—C38—C39—C40−0.2 (4)
C52—Ru3—P1—C26−167.34 (13)P1—C38—C39—C40173.0 (2)
Ru2—Ru3—P1—C26−48.60 (12)C38—C39—C40—C410.5 (4)
Ru1—Ru3—P1—C26−79.40 (10)C39—C40—C41—C42−0.9 (5)
C7—As1—C1—C228.7 (3)C40—C41—C42—C431.0 (5)
C13—As1—C1—C2−77.9 (2)C39—C38—C43—C420.3 (4)
Ru1—As1—C1—C2158.9 (2)P1—C38—C43—C42−173.3 (2)
C7—As1—C1—C6−153.4 (2)C41—C42—C43—C38−0.7 (5)
Hydrogen-bond geometry (Å, º) top
Cg1 and Cg2 are the centroids of the C1–C6 and C32–C37 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C10—H10A···O5i0.932.583.469 (4)160
C12—H12A···F2ii0.932.483.274 (3)143
C22—H22A···O4iii0.932.593.451 (5)154
C34—H34A···O4iv0.932.493.201 (4)134
C39—H39A···Cg1v0.932.933.749 (3)148
C41—H41A···Cg2vi0.932.733.607 (3)157
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+1, −y, −z; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y, −z+1; (v) x−1, y, z; (vi) −x, −y, −z+1.

Experimental details

Crystal data
Chemical formula[Ru3(C25H22As2)(C18H10F5P)(CO)9]·CHCl3
Mr1499.16
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)12.6354 (3), 14.1572 (3), 16.2418 (4)
α, β, γ (°)81.497 (1), 81.452 (1), 74.994 (1)
V (Å3)2756.86 (11)
Z2
Radiation typeMo Kα
µ (mm−1)2.25
Crystal size (mm)0.46 × 0.20 × 0.14
Data collection
DiffractometerBruker SMART APEXII CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2005)
Tmin, Tmax0.427, 0.745
No. of measured, independent and
observed [I > 2σ(I)] reflections		83481, 15949, 13916
Rint0.028
(sin θ/λ)max (Å−1)0.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.088, 1.07
No. of reflections15949
No. of parameters702
No. of restraints6
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)2.05, −1.70

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 the C1–C6 and C32–C37 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C10—H10A···O5i0.93002.58003.469 (4)160.00
C12—H12A···F2ii0.93002.48003.274 (3)143.00
C22—H22A···O4iii0.93002.59003.451 (5)154.00
C34—H34A···O4iv0.93002.49003.201 (4)134.00
C39—H39A···Cg1v0.93002.933.749 (3)148
C41—H41A···Cg2vi0.93002.733.607 (3)157
Symmetry codes: (i) −x+1, −y+1, −z; (ii) −x+1, −y, −z; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y, −z+1; (v) x−1, y, z; (vi) −x, −y, −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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ISSN: 2056-9890
Volume 66| Part 2| February 2010| Pages m176-m177
https://doi.org/10.1107/S1600536809055275
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