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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 2| February 2011| Pages m216-m217

[μ-Bis(di­phenyl­phosphan­yl)methane-1:2κ2P:P′]nona­carbonyl-1κ3C,2κ3C,3κ3C-[tris­­(bi­phenyl-4-yl)arsane-3κAs]-triangulo-triruthenium(0)

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 22 December 2010; accepted 6 January 2011; online 15 January 2011)

In the title triangulo-triruthenium compound, [Ru3(C36H27As)(C25H22P2)(CO)9], the bis­(diphenyl­phosphan­yl)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. In each biphenyl unit, the phenyl rings are twisted from each other, making dihedral angles of 51.22 (18), 42.94 (16) and 26.95 (16)°. The arsine-substituted phenyl rings make dihedral angles of 61.22 (15), 87.17 (15) and 83.32 (15)° with each other. The dihedral angles between the two benzene rings are 85.52 (18) and 81.77 (15)° for the two diphenyl­phosphanyl groups, respectively. In the crystal, mol­ecules are linked into dimers by inter­molecular C—H⋯O hydrogen bonds. Weak inter­molecular C—H⋯π and ππ [centroid–centroid distance = 3.6981 (18) Å] inter­actions 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. (2011a[Shawkataly, O. bin, Khan, I. A., Sirat, S. S., Yeap, C. S. & Fun, H.-K. (2011a). Acta Cryst. E67, o457-o458.],b[Shawkataly, O. bin, Khan, I. A., Sirat, S. S., Yeap, C. S. & Fun, H.-K. (2011b). Acta Cryst. E67, m214-m215.]). For the synthesis of Ru3(CO)10(μ-Ph2PCH2PPh2), 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 in 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(C36H27As)(C25H22P2)(CO)9]

  • Mr = 1474.16

  • Triclinic, [P \overline 1]

  • a = 10.8435 (7) Å

  • b = 12.6134 (8) Å

  • c = 22.4695 (15) Å

  • α = 81.029 (1)°

  • β = 82.769 (1)°

  • γ = 79.265 (1)°

  • V = 2967.6 (3) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 1.42 mm−1

  • T = 100 K

  • 0.50 × 0.17 × 0.02 mm

Data collection
  • Bruker APEXII DUO CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.539, Tmax = 0.967

  • 50392 measured reflections

  • 13475 independent reflections

  • 11159 reflections with I > 2σ(I)

  • Rint = 0.039

Refinement
  • R[F2 > 2σ(F2)] = 0.030

  • wR(F2) = 0.085

  • S = 1.11

  • 13475 reflections

  • 766 parameters

  • H-atom parameters constrained

  • Δρmax = 0.91 e Å−3

  • Δρmin = −0.67 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

Cg1 and Cg2 are the centroids of the C7–C12 and C26–C31 benzene rings, respectively.

D—H⋯A D—H H⋯A DA D—H⋯A
C46—H46A⋯O9i 0.93 2.56 3.249 (4) 131
C21—H21ACg1 0.93 2.95 3.707 (4) 139
C24—H24ACg2ii 0.93 2.92 3.582 (4) 129
Symmetry codes: (i) -x, -y+1, -z; (ii) x+1, y, z.

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). 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

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, herein we report the synthesis and structure of the title compound.

The bis(diphenylphosphanyl)methane ligand bridges the Ru1–Ru2 bond and the monodentate phosphine ligand bonds to the Ru3 atom. Both 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 (Fig 1). The conformation of the title compound is very identical to its closely related structure (Shawkataly et al., 2011b). Both phenyl rings of biphenyl (C26–C31/C32–C37, C38–C43/C44–C49 and C50–C55/C56–C61) make dihedral angles of 51.22 (18), 42.94 (16) and 26.95 (16)° from each other respectively are more twisted from each other compare to the reported monodentate arsine ligand (Shawkataly et al., 2011a). The arsine-substituted phenyl rings make dihedral angles (C26–C31/C38–C43, C26–C31/C50–C55 and C38–C43/C50–C55) of 61.22 (15), 87.17 (15) and 83.32 (15)° with each other respectively. The dihedral angles between the two benzene rings (C1–C6/C7–C12 and C14–C19/C20–C25) are 85.52 (18) and 81.77 (15)° for the two diphenylphosphanyl groups respectively.

In the crystal packing, the molecules are linked into dimers by intermolecular C46—H46A···O9 hydrogen bonds (Fig. 2, Table 1). Weak intermolecular C—H···π (Table 1) and Cg3···Cg3 interactions stabilize the crystal structure. Cg3···Cg3iii = 3.6981 (18) Å; Cg3 is centroid of C14–C19; (iii) 2 - x, -y, -z.

Related literature top

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985, 1988a,b). For related structures, see: Shawkataly et al. (2011a,b). For the synthesis of Ru3(CO)10(µ-Ph2PCH2PPh2), see: Bruce et al. (1983). For the stability of the temperature controller used in the data collection, see: Cosier & Glazer (1986).

Experimental top

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. Tri([1,1'-biphenyl]-4-yl)arsine is prepared by the reaction of AsCl3 with biphenyl magnesiumbromide in THF and Ru3(CO)10(µ-Ph2PCH2PPh2) (Bruce et al., 1983) was prepared by reported procedure. The title compound was obtained by refluxing equimolar quantities of Ru3(CO)10(µ-Ph2PCH2PPh2) and tri([1,1'-biphenyl]-4-yl)arsine in hexane under 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 or 0.97 Å and Uiso(H) = 1.2Ueq(C). The maximum and minimum residual electron density peaks of 0.91 and -0.67 e Å-3 were located 1.45 and 0.91 Å from the O8 and Ru1 atom, respectively.

Computing details top

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

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound with 50% probability ellipsoids for non-H atoms.
[Figure 2] Fig. 2. The crystal packing of the title compound, viewed down the b axis, showing the molecules are linked into dimers. Hydrogen atoms not involved in the hydrogen-bonding (dashed lines) have been omitted for clarity.
[µ-Bis(diphenylphosphanyl)methane-1:2κ2P:P']nonacarbonyl- 1κ3C,2κ3C,3κ3C-[tris(biphenyl-4-yl)arsane- 3κAs]-triangulo-triruthenium(0) top
Crystal data top
[Ru3(C36H27As)(C25H22P2)(CO)9]Z = 2
Mr = 1474.16F(000) = 1472
Triclinic, P1Dx = 1.650 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.8435 (7) ÅCell parameters from 9028 reflections
b = 12.6134 (8) Åθ = 2.8–29.9°
c = 22.4695 (15) ŵ = 1.42 mm1
α = 81.029 (1)°T = 100 K
β = 82.769 (1)°Plate, brown
γ = 79.265 (1)°0.50 × 0.17 × 0.02 mm
V = 2967.6 (3) Å3
Data collection top
Bruker APEXII DUO CCD area-detector
diffractometer
13475 independent reflections
Radiation source: fine-focus sealed tube11159 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
ϕ and ω scansθmax = 27.5°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2009)
h = 1314
Tmin = 0.539, Tmax = 0.967k = 1616
50392 measured reflectionsl = 2929
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)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.0394P)2 + 2.0751P]
where P = (Fo2 + 2Fc2)/3
13475 reflections(Δ/σ)max = 0.001
766 parametersΔρmax = 0.91 e Å3
0 restraintsΔρmin = 0.67 e Å3
Crystal data top
[Ru3(C36H27As)(C25H22P2)(CO)9]γ = 79.265 (1)°
Mr = 1474.16V = 2967.6 (3) Å3
Triclinic, P1Z = 2
a = 10.8435 (7) ÅMo Kα radiation
b = 12.6134 (8) ŵ = 1.42 mm1
c = 22.4695 (15) ÅT = 100 K
α = 81.029 (1)°0.50 × 0.17 × 0.02 mm
β = 82.769 (1)°
Data collection top
Bruker APEXII DUO CCD area-detector
diffractometer
13475 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2009)
11159 reflections with I > 2σ(I)
Tmin = 0.539, Tmax = 0.967Rint = 0.039
50392 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.085H-atom parameters constrained
S = 1.11Δρmax = 0.91 e Å3
13475 reflectionsΔρmin = 0.67 e Å3
766 parameters
Special details top

Experimental. The crystal was placed in the cold stream of an Oxford Cryosystems Cobra open-flow nitrogen cryostat (Cosier & Glazer, 1986) operating at 100.0 (1) K.

Geometry. All 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*/Ueq
Ru10.44891 (2)0.078490 (17)0.251421 (10)0.01666 (6)
Ru20.59682 (2)0.043132 (17)0.162673 (10)0.01608 (6)
Ru30.38778 (2)0.156754 (18)0.228718 (10)0.01686 (6)
As10.18353 (3)0.23145 (2)0.280389 (13)0.01803 (7)
P10.53340 (7)0.23935 (6)0.21184 (3)0.01721 (15)
P20.74739 (7)0.11370 (6)0.15430 (3)0.01714 (15)
O10.6635 (2)0.08213 (19)0.32987 (10)0.0307 (5)
O20.2964 (2)0.1792 (2)0.36158 (10)0.0366 (6)
O30.2224 (2)0.04572 (19)0.17687 (10)0.0306 (5)
O40.4449 (2)0.02871 (18)0.07405 (10)0.0278 (5)
O50.6747 (3)0.21237 (19)0.06021 (10)0.0377 (6)
O60.7332 (2)0.1412 (2)0.24679 (10)0.0315 (5)
O70.5071 (2)0.1390 (2)0.34769 (10)0.0325 (5)
O80.4815 (3)0.36584 (19)0.17562 (11)0.0404 (6)
O90.2679 (2)0.17734 (18)0.11014 (10)0.0300 (5)
C10.4231 (3)0.2927 (2)0.17412 (13)0.0214 (6)
C20.4389 (4)0.3083 (3)0.11416 (15)0.0347 (8)
H2A0.51040.29100.08990.042*
C30.3489 (4)0.3499 (3)0.08924 (17)0.0437 (10)
H3A0.36050.35930.04850.052*
C40.2444 (3)0.3767 (3)0.12452 (17)0.0345 (8)
H4A0.18640.40720.10840.041*
C50.2255 (4)0.3585 (3)0.18381 (18)0.0373 (9)
H5A0.15290.37460.20750.045*
C60.3125 (3)0.3169 (3)0.20871 (16)0.0329 (8)
H6A0.29780.30460.24890.040*
C70.5935 (3)0.3629 (2)0.26236 (13)0.0216 (6)
C80.6277 (3)0.4617 (2)0.23914 (14)0.0275 (7)
H8A0.61430.46540.19950.033*
C90.6816 (4)0.5544 (3)0.27470 (16)0.0383 (9)
H9A0.70490.61990.25880.046*
C100.7004 (4)0.5497 (3)0.33351 (16)0.0392 (9)
H10A0.73730.61180.35730.047*
C110.6646 (4)0.4525 (3)0.35749 (15)0.0346 (8)
H11A0.67620.45010.39750.041*
C120.6117 (3)0.3592 (3)0.32242 (14)0.0259 (7)
H12A0.58830.29420.33870.031*
C130.6680 (3)0.2300 (2)0.15242 (12)0.0190 (6)
H13A0.72890.29680.15750.023*
H13B0.63760.22360.11300.023*
C140.8514 (3)0.1181 (2)0.08339 (13)0.0201 (6)
C150.8004 (3)0.0690 (2)0.02949 (13)0.0237 (6)
H15A0.71680.03420.03040.028*
C160.8753 (3)0.0727 (3)0.02557 (13)0.0280 (7)
H16A0.84150.04070.06140.034*
C170.9990 (3)0.1235 (2)0.02698 (14)0.0278 (7)
H17A1.04900.12460.06380.033*
C181.0501 (3)0.1732 (3)0.02629 (15)0.0296 (7)
H18A1.13360.20830.02510.036*
C190.9754 (3)0.1701 (2)0.08146 (14)0.0249 (7)
H19A1.00930.20320.11710.030*
C200.8549 (3)0.1593 (2)0.21285 (13)0.0203 (6)
C210.8689 (3)0.2634 (3)0.24509 (14)0.0249 (6)
H21A0.82340.31360.23610.030*
C220.9496 (3)0.2942 (3)0.29044 (15)0.0312 (7)
H22A0.95730.36400.31190.037*
C231.0183 (3)0.2204 (3)0.30354 (15)0.0332 (8)
H23A1.07220.24080.33400.040*
C241.0076 (3)0.1164 (3)0.27177 (14)0.0302 (7)
H24A1.05430.06710.28070.036*
C250.9266 (3)0.0862 (3)0.22646 (14)0.0269 (7)
H25A0.91990.01650.20490.032*
C260.0712 (3)0.1451 (2)0.33399 (13)0.0214 (6)
C270.0586 (3)0.1666 (2)0.33179 (13)0.0240 (6)
H27A0.09410.22430.30470.029*
C280.1362 (3)0.1027 (3)0.36984 (13)0.0253 (7)
H28A0.22310.11850.36810.030*
C290.0847 (3)0.0155 (3)0.41026 (13)0.0260 (7)
C300.0441 (3)0.0045 (3)0.41272 (14)0.0303 (7)
H30A0.07960.06180.44000.036*
C310.1223 (3)0.0596 (3)0.37503 (14)0.0277 (7)
H31A0.20900.04480.37750.033*
C320.1695 (3)0.0550 (3)0.44874 (14)0.0280 (7)
C330.2758 (4)0.0132 (3)0.48258 (18)0.0440 (10)
H33A0.29720.06190.48200.053*
C340.3534 (4)0.0810 (4)0.51826 (19)0.0497 (11)
H34A0.42510.05040.54100.060*
C350.3249 (4)0.1900 (3)0.51981 (17)0.0426 (10)
H35A0.37510.23510.54430.051*
C360.2208 (5)0.2332 (3)0.48460 (19)0.0520 (11)
H36A0.20260.30800.48370.062*
C370.1421 (4)0.1665 (3)0.45017 (17)0.0418 (9)
H37A0.07000.19750.42780.050*
C380.0689 (3)0.3128 (2)0.22322 (13)0.0189 (6)
C390.0500 (3)0.4262 (2)0.21320 (14)0.0253 (7)
H39A0.08630.46390.23690.030*
C400.0220 (3)0.4828 (2)0.16844 (14)0.0255 (7)
H40A0.03210.55850.16180.031*
C410.0798 (3)0.4293 (2)0.13306 (13)0.0201 (6)
C420.0631 (3)0.3152 (2)0.14432 (14)0.0240 (6)
H42A0.10290.27770.12200.029*
C430.0116 (3)0.2581 (2)0.18805 (14)0.0238 (6)
H43A0.02380.18240.19410.029*
C440.1574 (3)0.4898 (2)0.08500 (13)0.0229 (6)
C450.1181 (3)0.5773 (3)0.04611 (14)0.0296 (7)
H45A0.04290.59890.05080.035*
C460.1900 (4)0.6326 (3)0.00051 (16)0.0387 (9)
H46A0.16320.69090.02520.046*
C470.3019 (4)0.6006 (3)0.00657 (17)0.0425 (9)
H47A0.34970.63670.03760.051*
C480.3424 (4)0.5159 (3)0.03199 (18)0.0432 (9)
H48A0.41880.49590.02760.052*
C490.2709 (3)0.4600 (3)0.07737 (15)0.0311 (7)
H49A0.29900.40210.10300.037*
C500.1957 (3)0.3424 (2)0.32999 (13)0.0206 (6)
C510.3039 (3)0.3891 (3)0.32329 (14)0.0270 (7)
H51A0.36960.36830.29440.032*
C520.3153 (3)0.4654 (3)0.35879 (14)0.0283 (7)
H52A0.38830.49600.35300.034*
C530.2209 (3)0.4978 (2)0.40296 (13)0.0244 (7)
C540.1089 (3)0.4544 (3)0.40785 (14)0.0293 (7)
H54A0.04190.47750.43560.035*
C550.0971 (3)0.3781 (3)0.37216 (14)0.0275 (7)
H55A0.02250.35010.37630.033*
C560.2393 (3)0.5731 (3)0.44450 (13)0.0276 (7)
C570.3587 (4)0.5795 (3)0.45740 (15)0.0357 (8)
H57A0.42780.53550.43980.043*
C580.3789 (4)0.6495 (3)0.49567 (16)0.0417 (9)
H58A0.46040.65270.50320.050*
C590.2778 (5)0.7135 (3)0.52219 (15)0.0448 (11)
H59A0.29040.75980.54850.054*
C600.1584 (4)0.7098 (3)0.51025 (15)0.0400 (10)
H60A0.09030.75400.52840.048*
C610.1373 (4)0.6409 (3)0.47137 (15)0.0353 (8)
H61A0.05560.63980.46320.042*
C620.5866 (3)0.0778 (2)0.29897 (13)0.0233 (6)
C630.3517 (3)0.1386 (2)0.31993 (13)0.0234 (6)
C640.3081 (3)0.0515 (2)0.20328 (13)0.0219 (6)
C650.4964 (3)0.0032 (2)0.10934 (13)0.0213 (6)
C660.6478 (3)0.1485 (2)0.09948 (13)0.0235 (6)
C670.6797 (3)0.1011 (2)0.21860 (13)0.0235 (6)
C680.4649 (3)0.1379 (2)0.30345 (14)0.0248 (7)
C690.4426 (3)0.2888 (2)0.19714 (14)0.0264 (7)
C700.3137 (3)0.1633 (2)0.15409 (14)0.0232 (6)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ru10.01510 (13)0.01704 (11)0.01680 (11)0.00413 (9)0.00168 (9)0.00005 (8)
Ru20.01274 (12)0.01755 (11)0.01752 (11)0.00462 (9)0.00147 (9)0.00097 (8)
Ru30.01466 (12)0.01714 (11)0.01768 (11)0.00304 (9)0.00072 (9)0.00051 (8)
As10.01521 (16)0.01817 (14)0.02020 (14)0.00388 (11)0.00016 (11)0.00104 (11)
P10.0151 (4)0.0171 (3)0.0187 (3)0.0043 (3)0.0000 (3)0.0001 (3)
P20.0133 (4)0.0192 (3)0.0186 (3)0.0041 (3)0.0008 (3)0.0017 (3)
O10.0280 (14)0.0378 (13)0.0279 (11)0.0057 (11)0.0070 (10)0.0052 (10)
O20.0341 (15)0.0388 (13)0.0309 (12)0.0096 (12)0.0090 (11)0.0085 (10)
O30.0235 (13)0.0353 (12)0.0332 (12)0.0119 (10)0.0074 (10)0.0071 (10)
O40.0234 (13)0.0366 (12)0.0258 (11)0.0082 (10)0.0042 (9)0.0064 (9)
O50.0469 (17)0.0292 (12)0.0332 (12)0.0144 (12)0.0128 (12)0.0034 (10)
O60.0218 (13)0.0428 (13)0.0350 (12)0.0111 (11)0.0034 (10)0.0141 (10)
O70.0280 (14)0.0446 (14)0.0262 (12)0.0020 (11)0.0055 (10)0.0117 (10)
O80.0486 (18)0.0282 (12)0.0440 (14)0.0193 (12)0.0108 (13)0.0008 (10)
O90.0346 (15)0.0286 (11)0.0248 (11)0.0020 (10)0.0102 (10)0.0004 (9)
C10.0194 (16)0.0156 (13)0.0292 (15)0.0046 (12)0.0030 (12)0.0010 (11)
C20.034 (2)0.046 (2)0.0302 (17)0.0238 (17)0.0013 (15)0.0046 (15)
C30.047 (3)0.059 (2)0.0349 (19)0.026 (2)0.0120 (18)0.0083 (17)
C40.0232 (19)0.0317 (17)0.053 (2)0.0069 (15)0.0106 (16)0.0100 (15)
C50.0218 (19)0.0364 (19)0.058 (2)0.0152 (15)0.0048 (17)0.0136 (17)
C60.027 (2)0.0382 (18)0.0358 (18)0.0144 (15)0.0078 (15)0.0107 (14)
C70.0156 (16)0.0218 (14)0.0248 (14)0.0038 (12)0.0014 (12)0.0026 (11)
C80.0291 (19)0.0225 (15)0.0275 (16)0.0002 (13)0.0019 (14)0.0015 (12)
C90.043 (2)0.0271 (17)0.0387 (19)0.0015 (16)0.0015 (17)0.0010 (14)
C100.040 (2)0.0328 (18)0.0362 (19)0.0029 (16)0.0016 (17)0.0102 (15)
C110.032 (2)0.0418 (19)0.0245 (16)0.0019 (16)0.0019 (14)0.0080 (14)
C120.0215 (17)0.0275 (15)0.0261 (15)0.0032 (13)0.0018 (13)0.0002 (12)
C130.0179 (16)0.0193 (13)0.0200 (13)0.0034 (12)0.0015 (11)0.0053 (11)
C140.0195 (16)0.0205 (13)0.0208 (13)0.0077 (12)0.0029 (12)0.0032 (11)
C150.0205 (17)0.0269 (15)0.0257 (15)0.0090 (13)0.0022 (12)0.0074 (12)
C160.035 (2)0.0340 (17)0.0186 (14)0.0147 (15)0.0006 (13)0.0056 (12)
C170.034 (2)0.0262 (15)0.0253 (15)0.0123 (14)0.0090 (14)0.0093 (12)
C180.0216 (18)0.0298 (16)0.0351 (17)0.0044 (14)0.0098 (14)0.0077 (13)
C190.0241 (18)0.0241 (15)0.0241 (15)0.0042 (13)0.0046 (13)0.0019 (12)
C200.0133 (15)0.0260 (14)0.0206 (14)0.0006 (12)0.0002 (11)0.0047 (11)
C210.0176 (16)0.0293 (16)0.0278 (15)0.0048 (13)0.0004 (13)0.0041 (12)
C220.0228 (18)0.0362 (18)0.0294 (16)0.0014 (14)0.0025 (14)0.0041 (14)
C230.0199 (18)0.052 (2)0.0256 (16)0.0000 (16)0.0037 (13)0.0055 (15)
C240.0190 (18)0.0442 (19)0.0297 (16)0.0073 (15)0.0018 (13)0.0137 (14)
C250.0192 (17)0.0348 (17)0.0272 (15)0.0067 (14)0.0010 (13)0.0060 (13)
C260.0227 (17)0.0219 (14)0.0195 (13)0.0066 (12)0.0025 (12)0.0026 (11)
C270.0219 (17)0.0239 (14)0.0254 (15)0.0041 (13)0.0028 (13)0.0007 (12)
C280.0177 (17)0.0309 (16)0.0281 (15)0.0075 (13)0.0003 (13)0.0038 (13)
C290.0270 (18)0.0278 (15)0.0238 (15)0.0113 (14)0.0040 (13)0.0029 (12)
C300.0278 (19)0.0318 (17)0.0285 (16)0.0064 (15)0.0037 (14)0.0066 (13)
C310.0167 (17)0.0321 (16)0.0310 (16)0.0017 (13)0.0007 (13)0.0013 (13)
C320.0276 (19)0.0350 (17)0.0219 (15)0.0112 (15)0.0025 (13)0.0015 (13)
C330.037 (2)0.039 (2)0.052 (2)0.0109 (18)0.0119 (19)0.0010 (17)
C340.033 (2)0.058 (3)0.052 (2)0.013 (2)0.0123 (19)0.005 (2)
C350.042 (2)0.048 (2)0.039 (2)0.0259 (19)0.0019 (18)0.0117 (17)
C360.062 (3)0.043 (2)0.049 (2)0.022 (2)0.008 (2)0.0050 (18)
C370.047 (3)0.0365 (19)0.0382 (19)0.0132 (18)0.0086 (18)0.0015 (15)
C380.0135 (15)0.0200 (13)0.0221 (14)0.0033 (11)0.0006 (11)0.0001 (11)
C390.0277 (18)0.0208 (14)0.0304 (16)0.0078 (13)0.0071 (14)0.0044 (12)
C400.0280 (19)0.0185 (14)0.0305 (16)0.0030 (13)0.0086 (14)0.0012 (12)
C410.0152 (15)0.0216 (14)0.0217 (14)0.0018 (12)0.0017 (11)0.0021 (11)
C420.0252 (18)0.0201 (14)0.0282 (15)0.0050 (13)0.0053 (13)0.0050 (12)
C430.0266 (18)0.0139 (13)0.0301 (16)0.0012 (12)0.0037 (13)0.0024 (11)
C440.0233 (17)0.0208 (14)0.0240 (14)0.0021 (12)0.0015 (12)0.0041 (11)
C450.031 (2)0.0273 (16)0.0302 (16)0.0067 (14)0.0062 (14)0.0001 (13)
C460.047 (3)0.0303 (17)0.0357 (19)0.0045 (17)0.0087 (17)0.0049 (14)
C470.050 (3)0.039 (2)0.039 (2)0.0014 (18)0.0252 (19)0.0024 (16)
C480.033 (2)0.045 (2)0.055 (2)0.0071 (18)0.0221 (19)0.0046 (18)
C490.0277 (19)0.0277 (16)0.0384 (18)0.0057 (14)0.0072 (15)0.0021 (14)
C500.0185 (16)0.0218 (14)0.0205 (13)0.0026 (12)0.0019 (12)0.0011 (11)
C510.0190 (17)0.0313 (16)0.0311 (16)0.0063 (13)0.0048 (13)0.0090 (13)
C520.0239 (18)0.0298 (16)0.0333 (17)0.0120 (14)0.0016 (14)0.0055 (13)
C530.0293 (19)0.0239 (14)0.0199 (14)0.0069 (13)0.0014 (13)0.0008 (11)
C540.0250 (19)0.0377 (18)0.0259 (15)0.0096 (15)0.0064 (13)0.0089 (13)
C550.0208 (18)0.0334 (17)0.0293 (16)0.0099 (14)0.0028 (13)0.0050 (13)
C560.036 (2)0.0253 (15)0.0207 (14)0.0082 (14)0.0017 (13)0.0024 (12)
C570.042 (2)0.0356 (18)0.0314 (17)0.0098 (17)0.0068 (16)0.0040 (14)
C580.058 (3)0.039 (2)0.0324 (18)0.0136 (19)0.0132 (18)0.0045 (15)
C590.081 (3)0.0333 (19)0.0253 (17)0.022 (2)0.0015 (19)0.0067 (14)
C600.058 (3)0.0360 (19)0.0258 (17)0.0155 (19)0.0133 (17)0.0085 (14)
C610.040 (2)0.0327 (17)0.0325 (17)0.0123 (16)0.0098 (16)0.0065 (14)
C620.0246 (18)0.0205 (14)0.0233 (14)0.0050 (13)0.0027 (13)0.0017 (11)
C630.0204 (17)0.0232 (14)0.0258 (15)0.0040 (13)0.0025 (13)0.0007 (12)
C640.0205 (17)0.0211 (14)0.0224 (14)0.0076 (12)0.0029 (12)0.0034 (11)
C650.0173 (16)0.0223 (14)0.0214 (14)0.0031 (12)0.0046 (12)0.0004 (11)
C660.0183 (16)0.0256 (15)0.0266 (15)0.0067 (13)0.0043 (12)0.0058 (12)
C670.0162 (16)0.0255 (15)0.0262 (15)0.0022 (12)0.0049 (12)0.0032 (12)
C680.0181 (17)0.0275 (15)0.0271 (16)0.0030 (13)0.0030 (13)0.0034 (12)
C690.0234 (18)0.0246 (15)0.0302 (16)0.0040 (13)0.0029 (13)0.0049 (12)
C700.0225 (17)0.0181 (13)0.0270 (15)0.0023 (12)0.0012 (13)0.0011 (11)
Geometric parameters (Å, º) top
Ru1—C631.892 (3)C22—H22A0.9300
Ru1—C641.930 (3)C23—C241.385 (5)
Ru1—C621.944 (3)C23—H23A0.9300
Ru1—P12.3265 (8)C24—C251.390 (5)
Ru1—Ru22.8389 (3)C24—H24A0.9300
Ru1—Ru32.8956 (4)C25—H25A0.9300
Ru2—C661.891 (3)C26—C311.384 (4)
Ru2—C671.933 (3)C26—C271.388 (5)
Ru2—C651.935 (3)C27—C281.395 (4)
Ru2—P22.3345 (8)C27—H27A0.9300
Ru2—Ru32.8285 (3)C28—C291.390 (4)
Ru3—C691.878 (3)C28—H28A0.9300
Ru3—C681.931 (3)C29—C301.379 (5)
Ru3—C701.932 (3)C29—C321.499 (4)
Ru3—As12.4612 (4)C30—C311.397 (4)
As1—C381.940 (3)C30—H30A0.9300
As1—C501.952 (3)C31—H31A0.9300
As1—C261.959 (3)C32—C331.365 (5)
P1—C11.826 (3)C32—C371.378 (5)
P1—C71.843 (3)C33—C341.402 (5)
P1—C131.858 (3)C33—H33A0.9300
P2—C201.823 (3)C34—C351.348 (6)
P2—C141.835 (3)C34—H34A0.9300
P2—C131.843 (3)C35—C361.370 (6)
O1—C621.139 (4)C35—H35A0.9300
O2—C631.150 (4)C36—C371.391 (5)
O3—C641.149 (4)C36—H36A0.9300
O4—C651.142 (4)C37—H37A0.9300
O5—C661.146 (4)C38—C431.393 (4)
O6—C671.138 (4)C38—C391.393 (4)
O7—C681.149 (4)C39—C401.378 (4)
O8—C691.145 (4)C39—H39A0.9300
O9—C701.136 (4)C40—C411.391 (4)
C1—C21.377 (4)C40—H40A0.9300
C1—C61.401 (4)C41—C421.403 (4)
C2—C31.400 (5)C41—C441.479 (4)
C2—H2A0.9300C42—C431.380 (4)
C3—C41.364 (5)C42—H42A0.9300
C3—H3A0.9300C43—H43A0.9300
C4—C51.371 (5)C44—C491.390 (5)
C4—H4A0.9300C44—C451.394 (4)
C5—C61.375 (5)C45—C461.385 (5)
C5—H5A0.9300C45—H45A0.9300
C6—H6A0.9300C46—C471.381 (6)
C7—C81.395 (4)C46—H46A0.9300
C7—C121.397 (4)C47—C481.370 (5)
C8—C91.385 (5)C47—H47A0.9300
C8—H8A0.9300C48—C491.382 (5)
C9—C101.374 (5)C48—H48A0.9300
C9—H9A0.9300C49—H49A0.9300
C10—C111.385 (5)C50—C511.389 (4)
C10—H10A0.9300C50—C551.394 (4)
C11—C121.381 (4)C51—C521.374 (4)
C11—H11A0.9300C51—H51A0.9300
C12—H12A0.9300C52—C531.384 (4)
C13—H13A0.9700C52—H52A0.9300
C13—H13B0.9700C53—C541.408 (4)
C14—C191.380 (4)C53—C561.485 (4)
C14—C151.401 (4)C54—C551.377 (4)
C15—C161.394 (4)C54—H54A0.9300
C15—H15A0.9300C55—H55A0.9300
C16—C171.373 (5)C56—C571.381 (5)
C16—H16A0.9300C56—C611.399 (5)
C17—C181.391 (5)C57—C581.386 (5)
C17—H17A0.9300C57—H57A0.9300
C18—C191.394 (4)C58—C591.365 (6)
C18—H18A0.9300C58—H58A0.9300
C19—H19A0.9300C59—C601.365 (6)
C20—C211.389 (4)C59—H59A0.9300
C20—C251.400 (4)C60—C611.390 (5)
C21—C221.389 (5)C60—H60A0.9300
C21—H21A0.9300C61—H61A0.9300
C22—C231.380 (5)
C63—Ru1—C6491.69 (13)C23—C22—C21119.6 (3)
C63—Ru1—C6291.95 (13)C23—C22—H22A120.2
C64—Ru1—C62169.84 (12)C21—C22—H22A120.2
C63—Ru1—P198.00 (9)C22—C23—C24120.6 (3)
C64—Ru1—P191.94 (9)C22—C23—H23A119.7
C62—Ru1—P196.94 (9)C24—C23—H23A119.7
C63—Ru1—Ru2168.92 (9)C23—C24—C25119.5 (3)
C64—Ru1—Ru293.18 (8)C23—C24—H24A120.3
C62—Ru1—Ru281.66 (8)C25—C24—H24A120.3
P1—Ru1—Ru291.782 (19)C24—C25—C20120.9 (3)
C63—Ru1—Ru3112.71 (9)C24—C25—H25A119.5
C64—Ru1—Ru376.03 (8)C20—C25—H25A119.5
C62—Ru1—Ru393.82 (9)C31—C26—C27118.9 (3)
P1—Ru1—Ru3147.04 (2)C31—C26—As1119.3 (2)
Ru2—Ru1—Ru359.098 (8)C27—C26—As1121.9 (2)
C66—Ru2—C6789.89 (13)C26—C27—C28120.7 (3)
C66—Ru2—C6590.22 (12)C26—C27—H27A119.7
C67—Ru2—C65173.34 (13)C28—C27—H27A119.7
C66—Ru2—P2105.29 (10)C29—C28—C27120.5 (3)
C67—Ru2—P296.30 (10)C29—C28—H28A119.8
C65—Ru2—P290.10 (9)C27—C28—H28A119.8
C66—Ru2—Ru3104.86 (10)C30—C29—C28118.5 (3)
C67—Ru2—Ru378.76 (9)C30—C29—C32122.0 (3)
C65—Ru2—Ru394.77 (9)C28—C29—C32119.5 (3)
P2—Ru2—Ru3149.428 (19)C29—C30—C31121.4 (3)
C66—Ru2—Ru1163.01 (10)C29—C30—H30A119.3
C67—Ru2—Ru196.62 (8)C31—C30—H30A119.3
C65—Ru2—Ru181.51 (8)C26—C31—C30120.1 (3)
P2—Ru2—Ru189.629 (19)C26—C31—H31A119.9
Ru3—Ru2—Ru161.450 (9)C30—C31—H31A119.9
C69—Ru3—C6895.45 (13)C33—C32—C37117.5 (3)
C69—Ru3—C7088.24 (13)C33—C32—C29122.5 (3)
C68—Ru3—C70175.47 (12)C37—C32—C29120.0 (3)
C69—Ru3—As198.37 (10)C32—C33—C34121.4 (4)
C68—Ru3—As190.29 (9)C32—C33—H33A119.3
C70—Ru3—As191.77 (10)C34—C33—H33A119.3
C69—Ru3—Ru289.80 (10)C35—C34—C33120.6 (4)
C68—Ru3—Ru296.06 (9)C35—C34—H34A119.7
C70—Ru3—Ru281.31 (9)C33—C34—H34A119.7
As1—Ru3—Ru2169.149 (12)C34—C35—C36118.8 (3)
C69—Ru3—Ru1147.65 (10)C34—C35—H35A120.6
C68—Ru3—Ru179.45 (9)C36—C35—H35A120.6
C70—Ru3—Ru196.03 (8)C35—C36—C37120.7 (4)
As1—Ru3—Ru1113.473 (11)C35—C36—H36A119.6
Ru2—Ru3—Ru159.452 (8)C37—C36—H36A119.6
C38—As1—C50101.53 (12)C32—C37—C36120.9 (4)
C38—As1—C26100.80 (13)C32—C37—H37A119.5
C50—As1—C26101.54 (12)C36—C37—H37A119.5
C38—As1—Ru3111.63 (9)C43—C38—C39118.8 (3)
C50—As1—Ru3113.18 (9)C43—C38—As1120.2 (2)
C26—As1—Ru3125.09 (9)C39—C38—As1120.9 (2)
C1—P1—C799.95 (13)C40—C39—C38120.4 (3)
C1—P1—C13102.47 (13)C40—C39—H39A119.8
C7—P1—C13102.02 (14)C38—C39—H39A119.8
C1—P1—Ru1114.45 (10)C39—C40—C41121.3 (3)
C7—P1—Ru1120.11 (10)C39—C40—H40A119.3
C13—P1—Ru1115.25 (9)C41—C40—H40A119.3
C20—P2—C14103.80 (14)C40—C41—C42118.0 (3)
C20—P2—C13105.34 (13)C40—C41—C44121.5 (3)
C14—P2—C13100.07 (12)C42—C41—C44120.5 (3)
C20—P2—Ru2118.69 (10)C43—C42—C41120.8 (3)
C14—P2—Ru2117.18 (10)C43—C42—H42A119.6
C13—P2—Ru2109.61 (10)C41—C42—H42A119.6
C2—C1—C6117.8 (3)C42—C43—C38120.6 (3)
C2—C1—P1125.0 (2)C42—C43—H43A119.7
C6—C1—P1117.2 (2)C38—C43—H43A119.7
C1—C2—C3120.9 (3)C49—C44—C45118.5 (3)
C1—C2—H2A119.5C49—C44—C41120.6 (3)
C3—C2—H2A119.5C45—C44—C41121.0 (3)
C4—C3—C2120.1 (3)C46—C45—C44120.7 (3)
C4—C3—H3A119.9C46—C45—H45A119.6
C2—C3—H3A119.9C44—C45—H45A119.6
C3—C4—C5119.6 (3)C47—C46—C45119.7 (3)
C3—C4—H4A120.2C47—C46—H46A120.2
C5—C4—H4A120.2C45—C46—H46A120.2
C4—C5—C6120.8 (3)C48—C47—C46120.1 (3)
C4—C5—H5A119.6C48—C47—H47A119.9
C6—C5—H5A119.6C46—C47—H47A119.9
C5—C6—C1120.7 (3)C47—C48—C49120.5 (4)
C5—C6—H6A119.7C47—C48—H48A119.7
C1—C6—H6A119.7C49—C48—H48A119.7
C8—C7—C12119.1 (3)C48—C49—C44120.4 (3)
C8—C7—P1119.1 (2)C48—C49—H49A119.8
C12—C7—P1121.8 (2)C44—C49—H49A119.8
C9—C8—C7120.5 (3)C51—C50—C55118.2 (3)
C9—C8—H8A119.8C51—C50—As1120.2 (2)
C7—C8—H8A119.8C55—C50—As1121.7 (2)
C10—C9—C8120.0 (3)C52—C51—C50120.9 (3)
C10—C9—H9A120.0C52—C51—H51A119.5
C8—C9—H9A120.0C50—C51—H51A119.5
C9—C10—C11120.1 (3)C51—C52—C53121.7 (3)
C9—C10—H10A119.9C51—C52—H52A119.2
C11—C10—H10A119.9C53—C52—H52A119.2
C12—C11—C10120.5 (3)C52—C53—C54117.4 (3)
C12—C11—H11A119.7C52—C53—C56120.9 (3)
C10—C11—H11A119.7C54—C53—C56121.7 (3)
C11—C12—C7119.8 (3)C55—C54—C53121.0 (3)
C11—C12—H12A120.1C55—C54—H54A119.5
C7—C12—H12A120.1C53—C54—H54A119.5
P2—C13—P1113.20 (14)C54—C55—C50120.7 (3)
P2—C13—H13A108.9C54—C55—H55A119.6
P1—C13—H13A108.9C50—C55—H55A119.6
P2—C13—H13B108.9C57—C56—C61117.6 (3)
P1—C13—H13B108.9C57—C56—C53120.8 (3)
H13A—C13—H13B107.8C61—C56—C53121.6 (3)
C19—C14—C15119.7 (3)C56—C57—C58122.1 (4)
C19—C14—P2122.4 (2)C56—C57—H57A118.9
C15—C14—P2117.9 (2)C58—C57—H57A118.9
C16—C15—C14119.8 (3)C59—C58—C57119.3 (4)
C16—C15—H15A120.1C59—C58—H58A120.4
C14—C15—H15A120.1C57—C58—H58A120.4
C17—C16—C15120.2 (3)C58—C59—C60120.2 (3)
C17—C16—H16A119.9C58—C59—H59A119.9
C15—C16—H16A119.9C60—C59—H59A119.9
C16—C17—C18120.4 (3)C59—C60—C61120.9 (4)
C16—C17—H17A119.8C59—C60—H60A119.5
C18—C17—H17A119.8C61—C60—H60A119.5
C17—C18—C19119.7 (3)C60—C61—C56119.9 (4)
C17—C18—H18A120.2C60—C61—H61A120.1
C19—C18—H18A120.2C56—C61—H61A120.1
C14—C19—C18120.3 (3)O1—C62—Ru1175.3 (3)
C14—C19—H19A119.8O2—C63—Ru1177.1 (3)
C18—C19—H19A119.8O3—C64—Ru1173.2 (2)
C21—C20—C25118.1 (3)O4—C65—Ru2174.2 (2)
C21—C20—P2123.0 (2)O5—C66—Ru2177.4 (3)
C25—C20—P2118.8 (2)O6—C67—Ru2173.4 (3)
C22—C21—C20121.3 (3)O7—C68—Ru3172.4 (3)
C22—C21—H21A119.4O8—C69—Ru3175.8 (3)
C20—C21—H21A119.4O9—C70—Ru3173.6 (3)
C63—Ru1—Ru2—C6682.9 (6)C13—P1—C7—C859.8 (3)
C64—Ru1—Ru2—C6633.1 (3)Ru1—P1—C7—C8171.3 (2)
C62—Ru1—Ru2—C66138.1 (3)C1—P1—C7—C12137.9 (3)
P1—Ru1—Ru2—C66125.1 (3)C13—P1—C7—C12116.9 (3)
Ru3—Ru1—Ru2—C6638.6 (3)Ru1—P1—C7—C1212.0 (3)
C63—Ru1—Ru2—C6729.0 (5)C12—C7—C8—C91.4 (5)
C64—Ru1—Ru2—C67144.98 (13)P1—C7—C8—C9175.4 (3)
C62—Ru1—Ru2—C6726.22 (13)C7—C8—C9—C100.7 (6)
P1—Ru1—Ru2—C67122.98 (10)C8—C9—C10—C110.6 (6)
Ru3—Ru1—Ru2—C6773.35 (9)C9—C10—C11—C121.1 (6)
C63—Ru1—Ru2—C65144.5 (5)C10—C11—C12—C70.4 (5)
C64—Ru1—Ru2—C6528.56 (13)C8—C7—C12—C110.9 (5)
C62—Ru1—Ru2—C65160.23 (13)P1—C7—C12—C11175.8 (3)
P1—Ru1—Ru2—C6563.47 (9)C20—P2—C13—P182.02 (18)
Ru3—Ru1—Ru2—C65100.20 (9)C14—P2—C13—P1170.52 (16)
C63—Ru1—Ru2—P2125.3 (5)Ru2—P2—C13—P146.75 (17)
C64—Ru1—Ru2—P2118.72 (9)C1—P1—C13—P2145.82 (16)
C62—Ru1—Ru2—P270.08 (9)C7—P1—C13—P2111.01 (17)
P1—Ru1—Ru2—P226.68 (3)Ru1—P1—C13—P220.87 (19)
Ru3—Ru1—Ru2—P2169.65 (2)C20—P2—C14—C1913.1 (3)
C63—Ru1—Ru2—Ru344.3 (5)C13—P2—C14—C1995.6 (3)
C64—Ru1—Ru2—Ru371.63 (9)Ru2—P2—C14—C19146.1 (2)
C62—Ru1—Ru2—Ru399.57 (9)C20—P2—C14—C15168.8 (2)
P1—Ru1—Ru2—Ru3163.67 (2)C13—P2—C14—C1582.6 (2)
C66—Ru2—Ru3—C6921.45 (14)Ru2—P2—C14—C1535.8 (2)
C67—Ru2—Ru3—C6965.41 (14)C19—C14—C15—C160.3 (4)
C65—Ru2—Ru3—C69112.95 (13)P2—C14—C15—C16178.5 (2)
P2—Ru2—Ru3—C69148.73 (11)C14—C15—C16—C170.5 (4)
Ru1—Ru2—Ru3—C69169.41 (10)C15—C16—C17—C181.1 (4)
C66—Ru2—Ru3—C68116.92 (13)C16—C17—C18—C190.8 (5)
C67—Ru2—Ru3—C6830.05 (13)C15—C14—C19—C180.6 (4)
C65—Ru2—Ru3—C68151.58 (12)P2—C14—C19—C18178.6 (2)
P2—Ru2—Ru3—C6853.27 (10)C17—C18—C19—C140.0 (5)
Ru1—Ru2—Ru3—C6873.95 (9)C14—P2—C20—C21102.9 (3)
C66—Ru2—Ru3—C7066.79 (13)C13—P2—C20—C211.8 (3)
C67—Ru2—Ru3—C70153.66 (12)Ru2—P2—C20—C21124.9 (2)
C65—Ru2—Ru3—C7024.71 (12)C14—P2—C20—C2577.4 (3)
P2—Ru2—Ru3—C70123.02 (9)C13—P2—C20—C25177.9 (2)
Ru1—Ru2—Ru3—C70102.34 (8)Ru2—P2—C20—C2554.7 (3)
C66—Ru2—Ru3—As1117.60 (12)C25—C20—C21—C221.3 (5)
C67—Ru2—Ru3—As1155.54 (11)P2—C20—C21—C22178.4 (2)
C65—Ru2—Ru3—As126.10 (10)C20—C21—C22—C230.6 (5)
P2—Ru2—Ru3—As172.22 (8)C21—C22—C23—C240.2 (5)
Ru1—Ru2—Ru3—As151.54 (6)C22—C23—C24—C250.2 (5)
C66—Ru2—Ru3—Ru1169.13 (10)C23—C24—C25—C200.5 (5)
C67—Ru2—Ru3—Ru1104.00 (9)C21—C20—C25—C241.2 (5)
C65—Ru2—Ru3—Ru177.63 (8)P2—C20—C25—C24178.4 (2)
P2—Ru2—Ru3—Ru120.68 (4)C38—As1—C26—C31167.7 (2)
C63—Ru1—Ru3—C69151.5 (2)C50—As1—C26—C3188.0 (3)
C64—Ru1—Ru3—C69122.5 (2)Ru3—As1—C26—C3141.4 (3)
C62—Ru1—Ru3—C6957.8 (2)C38—As1—C26—C2711.8 (3)
P1—Ru1—Ru3—C6951.18 (19)C50—As1—C26—C2792.4 (3)
Ru2—Ru1—Ru3—C6920.08 (19)Ru3—As1—C26—C27138.2 (2)
C63—Ru1—Ru3—C6868.06 (14)C31—C26—C27—C280.6 (5)
C64—Ru1—Ru3—C68153.99 (13)As1—C26—C27—C28179.0 (2)
C62—Ru1—Ru3—C6825.66 (13)C26—C27—C28—C290.6 (5)
P1—Ru1—Ru3—C68134.66 (10)C27—C28—C29—C301.4 (5)
Ru2—Ru1—Ru3—C68103.57 (9)C27—C28—C29—C32177.3 (3)
C63—Ru1—Ru3—C70112.19 (14)C28—C29—C30—C311.0 (5)
C64—Ru1—Ru3—C7026.27 (13)C32—C29—C30—C31177.7 (3)
C62—Ru1—Ru3—C70154.09 (13)C27—C26—C31—C301.0 (5)
P1—Ru1—Ru3—C7045.08 (10)As1—C26—C31—C30178.6 (2)
Ru2—Ru1—Ru3—C7076.18 (9)C29—C30—C31—C260.2 (5)
C63—Ru1—Ru3—As117.62 (10)C30—C29—C32—C33130.4 (4)
C64—Ru1—Ru3—As168.30 (9)C28—C29—C32—C3350.9 (5)
C62—Ru1—Ru3—As1111.34 (9)C30—C29—C32—C3750.5 (5)
P1—Ru1—Ru3—As1139.66 (4)C28—C29—C32—C37128.2 (4)
Ru2—Ru1—Ru3—As1170.752 (14)C37—C32—C33—C341.0 (6)
C63—Ru1—Ru3—Ru2171.63 (10)C29—C32—C33—C34179.9 (4)
C64—Ru1—Ru3—Ru2102.45 (9)C32—C33—C34—C350.3 (7)
C62—Ru1—Ru3—Ru277.91 (9)C33—C34—C35—C361.8 (7)
P1—Ru1—Ru3—Ru231.10 (4)C34—C35—C36—C373.2 (7)
C69—Ru3—As1—C3865.82 (13)C33—C32—C37—C360.4 (6)
C68—Ru3—As1—C38161.38 (12)C29—C32—C37—C36178.7 (4)
C70—Ru3—As1—C3822.65 (12)C35—C36—C37—C322.6 (7)
Ru2—Ru3—As1—C3872.69 (11)C50—As1—C38—C43165.2 (2)
Ru1—Ru3—As1—C38120.01 (9)C26—As1—C38—C4360.9 (3)
C69—Ru3—As1—C5047.98 (14)Ru3—As1—C38—C4374.0 (2)
C68—Ru3—As1—C5047.57 (13)C50—As1—C38—C3919.8 (3)
C70—Ru3—As1—C50136.46 (12)C26—As1—C38—C39124.1 (3)
Ru2—Ru3—As1—C50173.50 (11)Ru3—As1—C38—C39101.0 (2)
Ru1—Ru3—As1—C50126.18 (9)C43—C38—C39—C401.3 (5)
C69—Ru3—As1—C26172.52 (15)As1—C38—C39—C40173.8 (2)
C68—Ru3—As1—C2676.96 (14)C38—C39—C40—C411.4 (5)
C70—Ru3—As1—C2699.00 (14)C39—C40—C41—C420.2 (5)
Ru2—Ru3—As1—C2648.97 (13)C39—C40—C41—C44179.9 (3)
Ru1—Ru3—As1—C261.65 (11)C40—C41—C42—C431.9 (5)
C63—Ru1—P1—C175.39 (14)C44—C41—C42—C43178.4 (3)
C64—Ru1—P1—C116.59 (13)C41—C42—C43—C382.0 (5)
C62—Ru1—P1—C1168.35 (13)C39—C38—C43—C420.4 (5)
Ru2—Ru1—P1—C1109.84 (10)As1—C38—C43—C42175.5 (2)
Ru3—Ru1—P1—C183.52 (11)C40—C41—C44—C49137.7 (3)
C63—Ru1—P1—C743.49 (15)C42—C41—C44—C4942.1 (4)
C64—Ru1—P1—C7135.47 (14)C40—C41—C44—C4542.8 (4)
C62—Ru1—P1—C749.47 (14)C42—C41—C44—C45137.5 (3)
Ru2—Ru1—P1—C7131.28 (11)C49—C44—C45—C460.7 (5)
Ru3—Ru1—P1—C7157.60 (11)C41—C44—C45—C46178.9 (3)
C63—Ru1—P1—C13166.15 (15)C44—C45—C46—C470.0 (6)
C64—Ru1—P1—C13101.87 (13)C45—C46—C47—C481.1 (6)
C62—Ru1—P1—C1373.19 (14)C46—C47—C48—C491.5 (6)
Ru2—Ru1—P1—C138.63 (11)C47—C48—C49—C440.8 (6)
Ru3—Ru1—P1—C1334.95 (12)C45—C44—C49—C480.3 (5)
C66—Ru2—P2—C20110.86 (14)C41—C44—C49—C48179.2 (3)
C67—Ru2—P2—C2019.24 (14)C38—As1—C50—C51105.5 (3)
C65—Ru2—P2—C20158.89 (13)C26—As1—C50—C51150.8 (3)
Ru3—Ru2—P2—C2059.31 (12)Ru3—As1—C50—C5114.3 (3)
Ru1—Ru2—P2—C2077.38 (11)C38—As1—C50—C5573.7 (3)
C66—Ru2—P2—C1415.08 (15)C26—As1—C50—C5530.0 (3)
C67—Ru2—P2—C14106.69 (14)Ru3—As1—C50—C55166.6 (2)
C65—Ru2—P2—C1475.18 (13)C55—C50—C51—C522.3 (5)
Ru3—Ru2—P2—C14174.76 (10)As1—C50—C51—C52178.5 (3)
Ru1—Ru2—P2—C14156.68 (11)C50—C51—C52—C530.8 (5)
C66—Ru2—P2—C13128.13 (14)C51—C52—C53—C543.7 (5)
C67—Ru2—P2—C13140.25 (13)C51—C52—C53—C56174.6 (3)
C65—Ru2—P2—C1337.88 (12)C52—C53—C54—C553.4 (5)
Ru3—Ru2—P2—C1361.70 (11)C56—C53—C54—C55174.9 (3)
Ru1—Ru2—P2—C1343.63 (10)C53—C54—C55—C500.4 (5)
C7—P1—C1—C2110.8 (3)C51—C50—C55—C542.6 (5)
C13—P1—C1—C26.0 (3)As1—C50—C55—C54178.3 (3)
Ru1—P1—C1—C2119.5 (3)C52—C53—C56—C5725.7 (5)
C7—P1—C1—C670.9 (3)C54—C53—C56—C57152.6 (3)
C13—P1—C1—C6175.7 (3)C52—C53—C56—C61153.6 (3)
Ru1—P1—C1—C658.8 (3)C54—C53—C56—C6128.2 (5)
C6—C1—C2—C31.8 (5)C61—C56—C57—C580.3 (5)
P1—C1—C2—C3179.9 (3)C53—C56—C57—C58179.6 (3)
C1—C2—C3—C40.7 (6)C56—C57—C58—C590.8 (5)
C2—C3—C4—C52.7 (6)C57—C58—C59—C601.1 (5)
C3—C4—C5—C62.1 (6)C58—C59—C60—C610.3 (5)
C4—C5—C6—C10.4 (6)C59—C60—C61—C560.8 (5)
C2—C1—C6—C52.4 (5)C57—C56—C61—C601.1 (5)
P1—C1—C6—C5179.2 (3)C53—C56—C61—C60179.6 (3)
C1—P1—C7—C845.4 (3)
Hydrogen-bond geometry (Å, º) top
Cg1 and Cg2 are the centroids of the C7–C12 and C26–C31 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C46—H46A···O9i0.932.563.249 (4)131
C21—H21A···Cg10.932.953.707 (4)139
C24—H24A···Cg2ii0.932.923.582 (4)129
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Ru3(C36H27As)(C25H22P2)(CO)9]
Mr1474.16
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)10.8435 (7), 12.6134 (8), 22.4695 (15)
α, β, γ (°)81.029 (1), 82.769 (1), 79.265 (1)
V3)2967.6 (3)
Z2
Radiation typeMo Kα
µ (mm1)1.42
Crystal size (mm)0.50 × 0.17 × 0.02
Data collection
DiffractometerBruker APEXII DUO CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2009)
Tmin, Tmax0.539, 0.967
No. of measured, independent and
observed [I > 2σ(I)] reflections
50392, 13475, 11159
Rint0.039
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.085, 1.11
No. of reflections13475
No. of parameters766
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.91, 0.67

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

Hydrogen-bond geometry (Å, º) top
Cg1 and Cg2 are the centroids of the C7–C12 and C26–C31 benzene rings, respectively.
D—H···AD—HH···AD···AD—H···A
C46—H46A···O9i0.932.563.249 (4)131
C21—H21A···Cg10.932.953.707 (4)139
C24—H24A···Cg2ii0.932.923.582 (4)129
Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z.
 

Footnotes

Thomson Reuters ResearcherID: B-6034-2009. On secondment to: Multimedia University, Melaka Campus, Jalan Ayer Keroh Lama, 74750 Melaka, Malaysia.

§Thomson Reuters ResearcherID: E-2833-2010. Current address: Department of Chemistry, Gokhale Centenary College, Ankola 5813 14, NK, Karnataka, India.

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 Visiting Researcher position. SSS thanks USM for the G A position. HKF and CSY thank USM for the Research University Grant No. 1001/PFIZIK/811160.

References

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First citationShawkataly, O. bin, Khan, I. A., Sirat, S. S., Yeap, C. S. & Fun, H.-K. (2011b). Acta Cryst. E67, m214–m215.  Web of Science CSD CrossRef IUCr Journals Google Scholar
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Volume 67| Part 2| February 2011| Pages m216-m217
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