[μ-Bis(diphenyl­arsino)methane-1:2κ2As:As′]nona­carbonyl-1κ3C,2κ3C,3κ3C-[triphenyl­stibine-3κSb]-triangulo-triruthenium(0)

Shawkataly, O. bin; Khan, I.A.; Yeap, C.S.; Fun, H.-K.

doi:10.1107/S1600536809049927

Volume 66
Part 1
Pages m94-m95
January 2010

Received 12 November 2009
Accepted 20 November 2009
Online 24 December 2009

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.009 Å
R = 0.037
wR = 0.096
Data-to-parameter ratio = 18.8
Details

[-Bis(diphenylarsino)methane-1:2²As:As']nonacarbonyl-1³C,2³C,3³C-[triphenylstibine-3Sb]-triangulo-triruthenium(0)

Omar bin Shawkataly,^a ^*⁺ Imthyaz Ahmed Khan,^a Chin Sing Yeap ^b ⁺⁺ and Hoong-Kun Fun ^b ⁺⁺⁺

^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

In the title triangulo-triruthenium compound, [Ru₃(C₂₅H₂₂As₂)(C₁₈H₁₅Sb)(CO)₉], the bis(diphenylarsino)methane ligand bridges an Ru-Ru bond and the monodentate stibine ligand bonds to the third Ru atom. Both the stibine 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 three stibine-substituted phenyl rings make dihedral angles of 84.3 (3), 80.4 (3) and 70.5 (3)° with each other. The dihedral angles between the two phenyl rings are 85.9 (3) and 75.2 (3)° for the two diphenylarsine groups. In the crystal packing, molecules are linked into chains down the c axis via intermolecular C-HO hydrogen bonds. Weak intermolecular C-H [pi] interactions further stabilize the crystal structure.

Related literature

For general background to triangulo-triruthenium derivatives, see: Bruce et al. (1985, 1988a,b); Shawkataly et al. (1998, 2004, 2009). For related structures, see: Shawkataly et al. (2009). For the synthesis of [mu] -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

Crystal data

[Ru₃(C₂₅H₂₂As₂)(C₁₈H₁₅Sb)(CO)₉]
M_r = 1380.62
Monoclinic, C 2/c
a = 42.3464 (6) Å
b = 11.6246 (2) Å
c = 20.1185 (3) Å
= 91.823 (1)°
V = 9898.5 (3) Å³
Z = 8
Mo K radiation
= 2.82 mm^-1
T = 100 K
0.36 × 0.15 × 0.09 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005) T_min = 0.428, T_max = 0.796
55374 measured reflections
11349 independent reflections
8669 reflections with I > 2(I)
R_int = 0.042

Refinement

R[F² > 2(F²)] = 0.037
wR(F²) = 0.096
S = 1.08
11349 reflections
605 parameters
H-atom parameters constrained
_max = 1.45 e Å^-3
_min = -1.24 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C13-H13BO8ⁱ	0.97	2.59	3.290 (7)	129
C23-H23ACg1ⁱⁱ	0.93	2.88	3.686 (6)	146
C34-H34ACg2ⁱⁱⁱ	0.93	2.72	3.564 (6)	151
Symmetry codes: (i) $[x, -y+1, z-{\script{1\over 2}}]$ ; (ii) $[x, -y, z-{\script{3\over 2}}]$ ; (iii) $[-x, y, -z+{\script{1\over 2}}]$ . Cg1 and Cg2 are the centroids of the C14-C19 and C26-C31phenyl rings, respectively.

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

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SJ2682 ).

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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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.
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Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
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