[μ-Bis(diphenylarsino)methane-1:2κ2 As:As′]nonacarbonyl-1κ3 C,2κ3 C,3κ3 C-[triphenylstibine-3κSb]-triangulo-triruthenium(0)

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—H⋯O hydrogen bonds. Weak intermolecular C—H⋯π interactions further stabilize the crystal structure.

In the title triangulo-triruthenium compound, [Ru 3 (C 25 H 22 As 2 )(C 18 H 15 Sb)(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 Ru 3 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-HÁ Á ÁO hydrogen bonds. Weak intermolecular C-HÁ Á Á interactions further stabilize the crystal structure.
Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: SJ2682).

Experimental
All manipulations were performed under a dry oxygen-free dinitrogen atmosphere using standard Schlenk techniques, all solvents were dried over sodium and distilled from sodium benzophenone ketyl under nitrogen. Triphenylstibine (Fluka) used as received and µ-bis(diphenylarsino)methanedecacarbonyltriruthenium(0) (Bruce et al., 1983) was prepared by reported procedure. The title compound was obtained by refluxing equimolar quantities of Ru 3 (CO) 10 (µ-Ph 2 AsCH 2 AsPh 2 ) (105.5 mg, 0.1 mmol) and triphenylstibine (35.3 mg, 0.1 mmol) in hexane under nitrogen atmosphere. Crystals suitable for X-ray diffraction were grown by slow solvent / solvent diffusion of CH 3 OH into CH 2 Cl 2 .

Refinement
All hydrogen atoms were positioned geometrically and refined using a riding model with C-H = 0.93-0.97 Å and U iso (H) = 1.2 U eq (C). The final difference Fourier map reveals high peaks, ~1.5 e Å -3 , two of which are quite separate from the heavy atoms. These could be due to the presence of additional solvent, possibly methanol, and perhaps at partial occupancy.
Attempts to produce a satisfactory model of this solvent were not successful. Fig. 1. The molecular structure of the title compound with 30% probability ellipsoids for non-H atoms. [µ-Bis(diphenylarsino)methane-1:2κ 2 As:

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