Further studies on organonickel compounds: the synthesis of some new alkyl-, acyl- and cyclopentadienyl-derivatives and the crystal structure of trans-[Ni(CH2SiMe3)2(PMe3)2] |
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| Authors: | Ernesto Carmona Margarita Paneque Manuel L Poveda Robin D Rogers Jerry L Atwood |
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| Institution: | Departamento de Química Inorgánica, Facultad de Quimica, Universidad de Sevilla, Sevilla, Spain;Department of Chemistry, Northern Illinois University, Dekalb, IL 60115, U.S.A.;Department of Chemistry, University of Alabama, University, AL 35486, U.S.A. |
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| Abstract: | The complex NiCl2(PMe3)2] reacts with one equivalent of mg(CH2CMe3)Cl to yield the monoalkyl derivative trans-Ni(CH2CMe3)Cl(PMe3)2], which can be carbonylated at room temperature and pressure to afford the acyl Ni(COCH2CMe3)Cl(PMe3)2]. Other related alkyl and acyl complexes of composition Ni(R)(NCS)(PMe3)2] (R = CH2CMe3, COCH2CMe3) and Ni(R)(η-C5H5)L] (L = PMe3, R = CH2CMe3, COCH2CMe3; L = PPh3, R = CH2CMe2Ph) have been similarly prepared. Dialkyl derivatives NiR2(dmpe)] (R = CH2SiMe3, CH2CMe2Ph; dmpe = 1,2-bis(dimethylphosphine)ethane, Me2PCH2 CH2PMe2) have been obtained by phosphine replacement of the labile pyridine and NNN′N′-tetramethylethylenediamine ligands in the corresponding Ni(CH2SiMe3)2(py)2] and Ni(CH2CMe2Ph)2(tmen)] complexes. A single-crystal X-ray determination carried out on the previously reported trimethylphosphine derivative Ni(CH2SiMe3)2(PMe3)2] shows the complex belongs to the orthorhombic space group Pbcn, with a = 14.345(4), b = 12.656(3), c = 12.815(3) Å, Z = 4 and R 0.077 for 535 independent observed reflections. The phosphine ligands occupy mutually trans positions P-Ni-P 146.9(3)° in a distorted square-planar arrangement. |
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| Keywords: | Authors to whom correspondence should be addressed |
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