Structural studies on polynuclear osmium carbonyl hydrides: XXXIV. Elucidation of the molecular structure from a crystal structure of disordered (μ-H) 5Os 3Re(CO) 12

Abstract

The complex (μ-H) 5Os 3Re(CO) 12 crystallizes in the centrosymmetric hexagonal space group P6 3/ m ( C 2 6 h ; No. 176) with a 19.087(5), c 10.963(1) Å, V 3459(3) Å 3, and Z = 6. Diffraction data were collected on a Syntex P2 1 automated four-circle diffractometer (Mo- K α radiation, 2θ = 4.5–45.0°) and the structure was refined to R F = 7.9% for all 1480 unique reflections ( R F = 5.4% for those 1007 data with ¦ F o¦ > 6σ(¦ F o¦)). The molecule contains a tetrahedral core of metal atoms each associated with three terminal carbonyl ligands. It is bisected by a crystallographic mirror plane. Although the hydride ligands were not located, a consideration of metal-metal distances allows the distinction between osmium and rhenium atoms and suggests that the structure is subject to a subtle form of two-fold disorder.