Reactions of triosmium clusters with indole: X-ray structures of [Os3(CO)10(μ-OH)(μ-OMeCO)] and [Os3(μ-H)(CO)10(μ-1, 2-η2-NC8H6)

Abstract

Treatment of [Os3(CO)12] with indole in presence of a methanolic solution of Me3NO⋅2H2O at 60∘C afforded the previously reported compounds [(μ-H)Os3(CO)10(μ-OMe)] 2, [(μ-H)Os3(CO)10(μ-OH)] 3 and [Os3(CO)10(μ-OH)(μ-OMeCO)] 4 in 10, 5 and 20% yields, respectively. The reaction of [Os3(CO)10(MeCN)2] with indole at room temperature gave [(μ-H)Os3(CO)10(μ-1,2-η2-NC8H6)] 5 in 40% yield. Compounds 4 and 5 have been characterized by single crystal X-ray diffraction studies. Compound 4 crystallizes in the monoclinic space group P2(1)/c with a = 23.1239(3), b = 9.8087(4), c = 16.9017(6) A, β = 92.6998(14)∘, Z = 8 and V = 3829.3(2) A3 and 5 crystallizes in the monoclinic space group P2(1)/c with a = 9.009(3), b = 9.764(4), c = 24.906(6) A, β = 93.452(14)∘, Z = 4 and V = 2186.9(13) A3. Compound 4 consists of an open cluster of three osmium atoms with the hydroxy and methoxycarbonyl ligands bridging the open Os–Os edge. Compound 5 consists of an isosceles triangle of osmium atoms with one elongated Os–Os edge which is bridged by the hydride and the indolyl ligands.