(Benzyl­diphenyl­phosphine-3κP)[μ-bis(diphenyl­arsino)methane-1:2κ2As:As′]nona­carbonyl-1κ3C,2κ3C,3κ3C-triangulo-triruthenium(0)

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

doi:10.1107/S1600536809053045

Volume 66
Part 1
Pages m73-m74
January 2010

Received 7 December 2009
Accepted 9 December 2009
Online 16 December 2009

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.008 Å
R = 0.062
wR = 0.112
Data-to-parameter ratio = 23.7
Details

(Benzyldiphenylphosphine-3P)[-bis(diphenylarsino)methane-1:2²As:As']nonacarbonyl-1³C,2³C,3³C-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

The asymmetric unit of the title triangulo-triruthenium compound, [Ru₃(C₂₅H₂₂As₂)(C₁₉H₁₇P)(CO)₉], consists of two crystallographically independent molecules of the triangulo-triruthenium complex, A and B. The bis(diphenylarsino)methane ligand bridges an Ru-Ru bond and the monodentate phosphine ligand bonds to the third Ru atom. Both the phosphine and arsine ligands are equatorial with respect to the Ru₃ triangle. In addition, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. With regard to the three phosphine-substituted rings, the benzyl ring makes dihedral angles of 41.0 (3) and 43.9 (3)° with the other two benzene rings in molecule A; these angles are 49.8 (3) and 56.8 (3)° in molecule B. The dihedral angles between the two benzene rings are 76.1 (3) and 88.2 (3)° for the two diphenylarsino groups in molecule A and 71.3 (3) and 78.1 (3)° in molecule B. In the crystal packing, molecules are linked into chains 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). For related structures, see: Shawkataly et al. (1998, 2004, 2009). For the synthesis of [mu] -bis(diphenylarsino)methanedecacarbonyltriruthenium(0), see: Bruce et al. (1983). For stability of the temperature controller used for the data collection, see: Cosier & Glazer (1986).

Experimental

Crystal data

[Ru₃(C₂₅H₂₂As₂)(C₁₉H₁₇P)(CO)₉]
M_r = 1303.86
Monoclinic, P 2₁ /c
a = 13.4824 (2) Å
b = 35.5978 (6) Å
c = 23.3473 (4) Å
= 117.597 (1)°
V = 9930.5 (3) Å³
Z = 8
Mo K radiation
= 2.31 mm^-1
T = 100 K
0.48 × 0.16 × 0.03 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005) T_min = 0.402, T_max = 0.945
131198 measured reflections
29004 independent reflections
18757 reflections with I > 2(I)
R_int = 0.071

Refinement

R[F² > 2(F²)] = 0.062
wR(F²) = 0.112
S = 1.05
29004 reflections
1226 parameters
H-atom parameters constrained
_max = 2.08 e Å^-3
_min = -1.19 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C16A-H16AO6B	0.93	2.59	3.189 (6)	123
C30A-H30AO7Aⁱ	0.93	2.58	3.261 (6)	130
C42B-H42BO9Bⁱⁱ	0.93	2.58	3.241 (7)	129
C28A-H28ACg1ⁱⁱⁱ	0.93	2.72	3.570 (7)	152
C28B-H28BCg2^iv	0.93	2.87	3.648 (7)	142
C40A-H40ACg3	0.93	2.77	3.474 (7)	133
C44B-H44BCg4	0.93	2.94	3.615 (7)	130
Symmetry codes: (i) -x+2, -y+2, -z+1; (ii) -x, -y+1, -z+1; (iii) $[x+1, -y+{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (iv) $[x-1, -y+{\script{1\over 2}}, z-{\script{3\over 2}}]$ . Cg1, Cg2, Cg3 and Cg4 are the centroids of the C1B-C6B, C1A-C6A, C26A-C31A and C26B-C31B benzene 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: SJ2709 ).

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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