Abstract
Abstract The complex (μ-H) 3 Os 3 Rh(CO) 9 (η 6 -C 6 H 5 Me), previously synthesized by Shore and hsu has been subjected to a single-crystal X-ray structural analysis. The complex crystallizes in the centrosymmetric monoclinic space group C 2/ m (No. 12) with a 14.178(2), b 14.683(3), c 10.205(1) A, β 92.89(1)°, V 2121.6(6) A 3 and ϱ(calcd) 3.20 g cm −3 for mol. wt. 1020.78 and Z = 4. Diffraction data were collected with a Syntex P2 1 automated four-circle diffractometer (MO- K α : 2θ 4.0–50.0°) and the structure was solved and refined to R F 3.9% for all 1964 independent reflections ( R F 3.2% for those 1726 data with ¦ F 0 ¦ > 3σ(¦ F 0 ¦). All non-hydrogen atoms were located as were the three hydride ligands which bridge the three OsOs bonds. The η 6 -toluene ligand is bonded to the rhodium atom and is subject to a three-fold disorder; the entire molecule lies about a site of crystallographic C s ( m ) symmetry. The metal—metal distances in the tetrahedral cluster are Os(1)Os(1′) 2.88(1) A, Os(1)Os(2) = Os(1′)Os(2) = 2.888(1) A, Os(1)Rh = Os(1′)Rh = 2.702(1) A and Os(2)Rh 2.703(1) A.
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