Abstract
Treatment of the labile cluster Os3(CO)10(CH3CN)2 with morpholine in benzene at 60∘C afforded Os3(CO)10(μ-η2-NC4H6O)(μ-H) (1). Decarbonylation of 1 at 128∘C gave Os3(CO)9(μ3-η2-NC4H6O)(μ-H) (2), which reacts with PPh3 at ambient temperature to give an addition product Os3(CO)9(μ-η2-NC4H6O)(PPh3)(μ-H) (3). Compound 1 reacted with PPh3 at 98∘C to give the substitution product 4 which is an isomer of 3. The reaction of Ru3(CO)12 with morpholine in the presence of Me3NO in refluxing benzene at 80∘C afforded Ru3(CO)9(μ3-η2-NC4H6O)(μ-H) (5). Compounds 1– 5 have been characterized by elemental analysis, infrared, 1H NMR, and mass spectroscopic data. The molecular structure of 1 has been determined by single crystal X-ray diffraction analysis. Compound 1 crystallizes in the monoclinic space group P2/c with a = 29.598(8) A, b = 9.202(2) A, c = 14.496(4) A, β = 93.19(3)∘, Z = 8, and V = 3942(2) A3. Compound 1 consists of an isosceles triangle of osmium atoms with one elongated Os–Os edge, which is bridged by the hydride and the morpholine ligand.
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