The cations [Mo(CO)3(η7-C7H7)]+ and [Mo(η6-C6H5Me)(η7-C7H7)]+ react with an excess of acetylacetone in dry tetrahydrofuran to form the seventeen-electron aqua-complex [Mo(acac)(H2O)(η7-C7H7)]+, from which the water molecule may be displaced affording the species [Mo(acac)L(η7-C7H7)]+(L = PEt3, PMe2Ph, PMePh2, P(OMe)3, AsMe2Ph, or py). 1,2-Bis(diphenylphosphino)ethane (dppe) reacts with the aqua-complex to give a dimolybdenum dication [Mo2(acac)2(dppe)(η7-C7H7)2]2+. Crystals of the title compound are monoclinic, space group P21/n, with a= 8.664(9), b= 18.997(4), c= 9.625(13)Å, β= 112.39(8)°. The structure has been refined to R 0.059 (R′ 0.071) for 3 226 independent observed reflections to 2θ 65°(Mo-KαX-radiation) collected at ca. 215 K. All hydrogen atoms present have been located and positionally and thermally refined.
The crystal structure is built up of two pairs of [Mo(acac)(H2O)(η7-C7H7)]+ cations and [BF4]– anions surrounding a symmetry centre and linked via two independent H ⋯ F contacts of 1.84(9) and 2.07(12)Å. The cation features a formally MoI metal atom in an approximate octahedral geometry. The tetrafluoroboratecounter ion is essentially tetrehedral.
|Number of pages||7|
|Journal||Journal of the Chemical Society, Dalton Transactions|
|Publication status||Published - 1977|
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