Bis{[μ-bis­(diphenyl­phosphino)methane-1:2κ2P:P′]nona­carbonyl-1κ3C,2κ3C,3κ3C-[tris­(4-methoxy­phen­yl)arsine-3κAs]-triangulo-triruthenium(0)} dichloro­methane solvate

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

doi:10.1107/S1600536809052088

Volume 66
Part 1
Pages m30-m31
January 2010

Received 30 November 2009
Accepted 3 December 2009
Online 9 December 2009

Key indicators
Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.002 Å
Disorder in solvent or counterion
R = 0.023
wR = 0.055
Data-to-parameter ratio = 34.2
Details

Bis{[-bis(diphenylphosphino)methane-1:2²P:P']nonacarbonyl-1³C,2³C,3³C-[tris(4-methoxyphenyl)arsine-3As]-triangulo-triruthenium(0)} dichloromethane solvate

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, 2[Ru₃(C₂₁H₂₁AsO₃)(C₂₅H₂₂P₂)(CO)₉]·CH₂Cl₂, contains one triangulo-triruthenium complex molecule and one half-molecule of the dichloromethane solvent. The dichloromethane solvent lies across a crystallographic inversion center leading to the molecule being disordered over two positions of equal occupancy. The bis(diphenylphosphino)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. The three arsine-substituted benzene rings make dihedral angles of 82.00 (6), 76.67 (7) and 66.09 (6)° with each other. The dihedral angles between the two benzene rings are 80.12 (8) and 78.34 (7)° for the two diphenylphosphino groups. In the crystal packing, the molecules are linked together into chains down the b axis via intermolecular C-HO hydrogen bonds. An intermolecular C-HO hydrogen bond and 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 tris(4-methoxyphenyl)arsine, see: Blicke & Cataline (1938) and for that of [mu] -bis(diphenylphosphino)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

2[Ru₃(C₂₁H₂₁AsO₃)(C₂₅H₂₂P₂)(CO)₉]·CH₂Cl₂
M_r = 2756.85
Triclinic, $[P \overline 1]$
a = 10.7428 (1) Å
b = 12.6731 (1) Å
c = 20.6529 (2) Å
= 95.523 (1)°
= 101.315 (1)°
= 103.929 (1)°
V = 2645.47 (4) Å³
Z = 1
Mo K radiation
= 1.64 mm^-1
T = 100 K
0.30 × 0.23 × 0.14 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005) T_min = 0.637, T_max = 0.797
123575 measured reflections
23203 independent reflections
20247 reflections with I > 2(I)
R_int = 0.030

Refinement

R[F² > 2(F²)] = 0.023
wR(F²) = 0.055
S = 1.02
23203 reflections
679 parameters
H-atom parameters constrained
_max = 1.72 e Å^-3
_min = -1.34 e Å^-3

Table 1
Hydrogen-bond geometry (Å, °)

D-HA	D-H	HA	DA	D-HA
C53-H53CO2ⁱ	0.96	2.60	3.346 (2)	135
C56-H56AO7	0.96	2.60	3.116 (3)	114
C22-H22ACg1ⁱⁱ	0.93	2.91	3.5901 (16)	131
C53-H53BCg2ⁱⁱⁱ	0.96	2.85	3.6951 (17)	147
Symmetry codes: (i) x, y+1, z; (ii) x-1, y, z; (iii) -x+2, -y+2, -z+1. Cg1 and Cg2 are the centroids of theC32-C37 and C26-C31 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: SJ2701 ).

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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