[μ-Bis(diphenyl­arsino)methane-1:2κ2As:As′]nona­carbonyl-1κ3C,2κ3C,3κ3C-[tris­(4-methyl­phen­yl)­phosphine-3κP]-triangulo-triruthenium(0)

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

doi:10.1107/S1600536809049940

Volume 66
Part 1
Pages m36-m37
January 2010

Received 12 November 2009
Accepted 20 November 2009
Online 9 December 2009

Key indicators
Single-crystal X-ray study
T = 296 K
Mean (C-C) = 0.007 Å
R = 0.049
wR = 0.096
Data-to-parameter ratio = 24.8
Details

[-Bis(diphenylarsino)methane-1:2²As:As']nonacarbonyl-1³C,2³C,3³C-[tris(4-methylphenyl)phosphine-3P]-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)(C₂₁H₂₁P)(CO)₉], the bis(diphenylarsino)methane ligand bridges a 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. Additionally, each Ru atom carries one equatorial and two axial terminal carbonyl ligands. The three phenyl rings of the phosphine make dihedral angles of 86.89 (19), 82.1 (2) and 63.0 (2)° with each other. The dihedral angles between the two phenyl rings are 73.8 (2) and 82.2 (3)° for the two diphenylarsino groups. An intramolecular C-HO hydrogen bond stabilizes the molecular structure. In the crystal packing, molecules are linked into chains down the b axis via intermolecular C-HO hydrogen bonds.

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 in the data collection, see: Cosier & Glazer (1986).

Experimental

Crystal data

[Ru₃(C₂₅H₂₂As₂)(C₂₁H₂₁P)(CO)₉]
M_r = 1331.91
Monoclinic, P 2₁ /c
a = 16.2585 (2) Å
b = 16.9247 (2) Å
c = 19.6900 (2) Å
= 98.680 (1)°
V = 5356.05 (11) Å³
Z = 4
Mo K radiation
= 2.15 mm^-1
T = 296 K
0.21 × 0.21 × 0.03 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005) T_min = 0.665, T_max = 0.933
63277 measured reflections
15703 independent reflections
9536 reflections with I > 2(I)
R_int = 0.063

Refinement

R[F² > 2(F²)] = 0.049
wR(F²) = 0.096
S = 1.00
15703 reflections
634 parameters
H-atom parameters constrained
_max = 0.60 e Å^-3
_min = -0.41 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C27-H27AO9	0.93	2.57	3.317 (5)	138
C54-H54AO2ⁱ	0.96	2.60	3.306 (6)	131
Symmetry code: (i) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ .

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: SJ2681 ).

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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Bruker (2005). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
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Spek, A. L. (2009). Acta Cryst. D65, 148-155.