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Título: | Synthesis and reactivity of half-sandwich (eta(5)-C(5) Me(5))Ir(III)complexes of a cyclometallated aryl phosphine ligand |
Autor: | Campos, Jesús CSIC ORCID CVN; Álvarez, Eleuterio CSIC ORCID ; Carmona, Ernesto CSIC ORCID | Fecha de publicación: | 2011 | Editor: | Royal Society of Chemistry (UK) | Citación: | New Journal of Chemistry 35: 2122- 2129 (2011) | Resumen: | Reaction of the Ir(III) dimer [(η5-C5Me5)IrCl2]2 with PMeXyl2 (Xyl = 2,6-C6H3Me2), in the presence of the poorly coordinating base 2,2,6,6-tetramethyl piperidine, gives a chloride complex 1-Cl, resulting from hydrogen chloride elimination involving one of the phosphine benzylic hydrogen atoms and concomitant cyclometallation . Related compounds containing other halide or pseudohalide ligands, 1-Br, 1-Cl, 1-SCN, can be made, the latter featuring S-coordination of the ambidentate thiocyanate to the soft Ir(III) Lewis acid centre, as suggested by IR data and demonstrated by X-ray crystallography . Hydride 2-H, and alkyl derivatives 3 (Me) and 4 (CH2SiMe3) can also be prepared from 1-Cl and appropriate hydride and alkylating reagents. An interesting H/D exchange chemistry that occurs in the presence of CD3OD has been disclosed for 1-Cl, 1-Br and 2-H. For the halide derivatives, deuterium incorporation takes place into the methylene and methyl sites of their cyclometallated ligand, whereas for 2-H only the hydride and methylene (Ir–CH2) protons participate in the exchange, which is strikingly accelerated by catalytic amounts of acids. | URI: | http://hdl.handle.net/10261/75384 | DOI: | 10.1039/C1NJ20244H | Identificadores: | doi: 10.1039/C1NJ20244H issn: 1144-0546 |
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