E. Shestakova, Y. Varshavsky, V. Khrustalev
Jul 1, 2013
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Journal
Journal of Organometallic Chemistry
Abstract
Abstract The rhodium(III) cationic methyl acetamidine complex, trans -[Rh(Acac)(PPh 3 ) 2 (CH 3 ){NH C(NH 2 )CH 3 }][BPh 4 ], ( 1 ) is formed upon the reaction of trans -[Rh(Acac)(PPh 3 ) 2 (CH 3 )(CH 3 CN)][BPh 4 ] with ammonia gas in CH 2 Cl 2 solution at temperatures between −15 °C and −20 °C. Complex 1 was characterized by elemental analysis, 31 P{ 1 H} and 1 H NMR spectra, and single crystal X-ray diffraction study. The cation of 1 has a slightly distorted octahedral structure. The equatorial plane contains the acetylacetonate, methyl, and acetamidine ligands; two PPh 3 ligands occupy the axial positions . The acetamidine ligand adopts the Z -configuration stabilized by hydrogen bonding with the oxygen atom of the acetylacetonate ligand, HN–H⋯O (1.90 A). Complex 1 reacts with ammonia gas at temperatures between 0 °C and 20 °C to form cationic monophosphine complex [Rh(Acac)(PPh 3 )(CH 3 ){NH C(NH 2 )CH 3 }(NH 3 )][BPh 4 ] ( 2 ). Complex 2 was characterized by 31 P{ 1 H} and 1 H NMR spectra without isolation.