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One-Pot Synthesis of Metal Primary Phosphine Complexes from OPCl2R or PCl2R. Isolation and Characterization of Primary Alkylphosphine Complexes of a Metalloporphyrin

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posted on 24.07.2006, 00:00 by Jie-Sheng Huang, Guang-Ao Yu, Jin Xie, Nianyong Zhu, Chi-Ming Che
Treatment of [RuII(Por)(CO)] [Por = porphyrinato(2−)] and OPCl2R [R = Ad (adamantyl), But, Busec] or PCl2Mes (Mes = mesityl) with LiAlH4 afforded primary alkyl- and arylphosphine complexes [RuII(Por)(PH2R)2], which have been isolated in pure form and characterized by 1H NMR, 31P NMR, IR, and UV−vis spectroscopy and mass spectrometry. The structures of [RuII(TTP)(PH2Ad)2] and [RuII(F20-TPP)(PH2Mes)2] were determined by X-ray crystallography.