Undecacarbonyl-1κ3 C,2κ4 C,3κ4 C-[tris(2-chloroethyl) phosphite-1κP]-triangulo-triruthenium(0)

In the title triangulo-triruthenium compound, [Ru3(C6H12Cl3O3P)(CO)11], one equatorial carbonyl ligand is substituted by a monodentate phosphite ligand, leaving one equatorial and two axial carbonyl ligands on one Ru atom. The remaining two Ru atoms each carry two equatorial and two axial terminal carbonyl ligands. In the crystal structure, the molecules are linked into a one-dimensional column along [100] by intermolecular C—H⋯O hydrogen bonds.

In the title triangulo-triruthenium compound, [Ru 3 (C 6 H 12 -Cl 3 O 3 P)(CO) 11 ], one equatorial carbonyl ligand is substituted by a monodentate phosphite ligand, leaving one equatorial and two axial carbonyl ligands on one Ru atom. The remaining two Ru atoms each carry two equatorial and two axial terminal carbonyl ligands. In the crystal structure, the molecules are linked into a one-dimensional column along [100] by intermolecular C-HÁ Á ÁO hydrogen bonds.
The monodentate phosphite ligand is bonded equatorially to the Ru1 atoms of the triangulo-triruthenium unit. Thus, the Ru2 and Ru3 atoms each carry two equatorial and two axial terminal carbonyl ligands, while the phosphite-bonded Ru1 atom binds one equatorial and two axial terminal carbonyl ligands.
In the crystal structure, the molecules are linked into a one-dimensional column along [1 0 0] by intermolecular C-H···O hydrogen bonds (Fig. 2, Table 1).

Experimental
All the manipulations were performed under a dry oxygen-free nitrogen atmosphere using standard Schlenk techniques. THF was dried over sodium wire and freshly distilled from sodium benzophenone ketyl solution. The title compound was prepared by mixing Ru 3 (CO) 12 (Aldrich) and P(OCH 2 CH 2 Cl) 3 (Maybridge) in a 1:1 molar ratio in THF at 40°C. Diphenylketyl radical anion initiator of about 0.2 ml (synthesized as per the method of Bruce et al., 1987) was introduced into the reaction mixture under a current of nitrogen. After stirring of 15 min, the solvent was removed under vacuum. Separation of the product in a pure form was done by column chromatography (Florisil, 100-200 mesh; eluant, dichloromethane: hexane).
Crystals suitable for X-ray diffraction were grown by slow diffusion of CH 3 OH into the CH 2 Cl 2 solution.

Refinement
H atoms were positioned geometrically and refined using a riding model, with C-H = 0.97 Å and U iso (H) = 1.2U eq (C).
The maximum and minimum residual electron density peaks of 1.36 and -1.36 eÅ -3 were located 1.32 and 0.81 Å from the C8 and Ru3 atoms, respectively. Fig. 1. The molecular structure of the title compound with 50% probability ellipsoids for non-H atoms.