Hydroboration of (μ-H)2Os3(CO)10: Formation of the Borylidyne Cluster (μ-H)2Os3(CO)9(μ-H)2BH. An Improved Synthesis of (μ-H)3Os3(CO)9(μ3-BCO)†
journal contributionposted on 08.10.1997, 00:00 by Jang-Hoon Chung, Edwin P. Boyd, Jianping Liu, Sheldon G. Shore
At room temperature, the reaction of (μ-H)2Os3(CO)10 with BH3S(CH3)2 produces the new borylidyne cluster (μ-H)2Os3(CO)9(μ-H)2BH, a methylidyne cluster analog. At 65 °C the previously reported ketenylidene cluster analog (μ-H)3Os3(CO)9(μ3-BCO) is formed. The complex (μ-H)2Os3(CO)9(μ-H)2BH was characterized by 1H NMR, 11B NMR, and infrared spectroscopies as well as mass spectrometry. Its molecular structure was determined from a single-crystal X-ray analysis. The molecule is of approximate Cs symmetry. It consists of a tetrahedral Os3B core with a terminal B−H bond, two Os−H−B, hydrogen bridge bonds, and three Os(CO)3 units. A similar structure has been proposed for one of the isomers of a ruthenium analog, (μ-H)2Ru3(CO)9(μ-H)2BH, but it differs from the related iron complex (μ-H)Fe3(CO)9(μ-H)3BH which has three Fe−H−B bridge bonds. Crystal data for (μ-H)2Os3(CO)9(μ-H)2BH: triclinic space group P1̄, a = 9.501(4) Å, b = 9.525(4) Å, c = 10.070(2) Å, α = 87.72(3) β = 88.32(3)°, γ = 61.45(3)°, Z = 2.