High oxidation state organometallics. Pentamethylcyclopentadienyloxo-molybdenum(VI) and -tungsten(VI) complexes

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Abstract

The preparation, isolation, and characterization of [(η5-C5Me5)MoO2]2O (1) and (η5-C5Me5)MoO2Cl (2) and their tungsten analogues (1′ and 2′) are described. A substantial improvement in stability, ease of preparation, and ease of separation from other reaction products are observed for these Cp* complexes compared to their cyclopentadienyl counterparts. The binuclear pentaoxo compound, 1, crystallizes in the monoclinic space group P21c with one and a half molecules in the asymmetric unit, Z = 6, a 21.265(7), b 9.237(3), c 17.669(5) Å, β 101.78(3)°, and V 3398(4) Å3. Anisotropic refinement of the molybdenum and isotropic refinement of the non-metal atoms with no hydrogen atoms included converged to the residuals R1 = 0.075, R2 = 0.088. Two independent μ-oxo complexes are represented in the cell: one is centrosymmetric having the bridging oxygen on a special position: and the other nearly centrosymmetric having a MoOMo angle of 177.9(5)°. Grignard addition to 2′ yields the air-stable alkyl, (η5-C5Me5)WO2CH2SiMe3.

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