Structural studies on osmium carbonyl hydrides: XXXI. Crystal and molecular structure of CpWOs 3(CO) 9(μ-H)(μ-O)(μ-CHCH 2C 6H 4Me), a hydrido-alkylidene produced by hydrogenation of a μ 3-alkylidyne

Abstract

The complex CpWOs 3(CO) 9(μ-H)(μ-O)(μ-CHCH 2C 6H 4Me), previously prepared by hydrogenation of CpWOs 3(CO) 9(μ-O)(μ 3-CCH 2C 6H 4Me), has been subjected to a single-crystal X-ray diffraction study. The complex crystallizes in the non-centrosymmetric monoclinic space group Cc( C s 4; No. 9) with a 14.1510(27), b 13.9257(22), c 13.3179(19) Å, β 92.023(13)°, V 2622.8(7) Å 3 and D(calcd) 3.06 g cm −3 for Z = 4 and mol. wt. 1206.8. Single-crystal X-ray diffraction data were collected with a Syntex P2 1 automated four-circle diffractometer and the structure was refined to R 3.5% for all 2476 independent observations (Mo- K α radiation, 2θ = 4.5–40.0°) and R 3.4% for those 2430 data with | F 0| > 3.0σ(| F 0|). The molecule contains a tetrahedral WOs 3 core associated with 60 valence electrons. Each osmium atom is associated with three terminal carbonyl ligands and the tungsten atom is linked to an η 5-C 5H 5 ligand. In addition, the μ-oxo ligand is involved in a WO: → Os bridge (in which WO(B) 1.737(17), Os(3)← :O(B) 2.167(16) Å and WO(B)Os(3) 96.0(7)°), the μ-hydride ligand spans the Os(1)Os(3) linkage and the μ-CHCH 2C 6H 4Me ligand bridges the WOs(2) linkage (WC(1) 2.068(26) and Os(2)C(1) 2.281(26) Å).