Preparation of benzophenone imine complexes of transition metals

Benzophenone imine [ M ( η 1 -NH CPh 2 ) ( CO ) n P 5 - n ] BPh 4 [M = Mn, Re; n = 2, 3; P = P(OEt)3, PPh(OEt)2, PPh2OEt, PPh3] complexes were prepared by allowing triflate M ( κ 1 -OTf ) ( CO ) n P 5 - n compounds to react with an excess of the imine. Hydride-imine [ MH ( η 1 -NH CPh 2 ) P 4 ] BPh 4 (M = Ru, Os), triflate-imine [ Os ( κ 1 -OTf ) ( η 1 -NH CPh 2 ) P 4 ] BPh 4 and bis(imine) [ Ru ( η 1 -NH CPh 2 ) 2 P 4 ] ( BPh 4 ) 2 [P = P(OEt)3] derivatives were also prepared. The complexes were characterized spectroscopically (IR, 1H, 31P, 13C NMR) and a geometry in solution was also established. Hydride-benzophenone imine [ IrHCl ( η 1 -NH CPh 2 ) L ( PPh 3 ) 2 ] BPh 4 and [ IrHCl ( η 1 -NH CPh 2 ) L ( AsPh 3 ) 2 ] BPh 4 [L = P(OEt)3 and PPh(OEt)2] complexes were prepared by reacting hydride IrHCl 2 L ( PPh 3 ) 2 and IrHCl 2 L ( AsPh 3 ) 2 precursors with an excess of imine. Dihydride IrH 2 ( η 1 -NH CPh 2 ) ( PPh 3 ) 3 complex was also obtained and a geometry in solution was proposed.