Preparation of benzophenone imine complexes of transition metals

Benzophenone imine [M(η1-NHCPh2)(CO)nP5-n]BPh4[M(η1-NHCPh2)(CO)nP5-n]BPh4 [M = Mn, Re; n = 2, 3; P = P(OEt)3, PPh(OEt)2, PPh2OEt, PPh3] complexes were prepared by allowing triflate M(κ1-OTf)(CO)nP5-nM(κ1-OTf)(CO)nP5-n compounds to react with an excess of the imine. Hydride-imine [MH(η1-NHCPh2)P4]BPh4[MH(η1-NHCPh2)P4]BPh4 (M = Ru, Os), triflate-imine [Os(κ1-OTf)(η1-NHCPh2)P4]BPh4[Os(κ1-OTf)(η1-NHCPh2)P4]BPh4 and bis(imine) [Ru(η1-NHCPh2)2P4](BPh4)2[Ru(η1-NHCPh2)2P4](BPh4)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(η1-NHCPh2)L(PPh3)2]BPh4[IrHCl(η1-NHCPh2)L(PPh3)2]BPh4and [IrHCl(η1-NHCPh2)L(AsPh3)2]BPh4[IrHCl(η1-NHCPh2)L(AsPh3)2]BPh4 [L = P(OEt)3 and PPh(OEt)2] complexes were prepared by reacting hydride IrHCl2L(PPh3)2IrHCl2L(PPh3)2 and IrHCl2L(AsPh3)2IrHCl2L(AsPh3)2 precursors with an excess of imine. Dihydride IrH2(η1-NHCPh2)(PPh3)3IrH2(η1-NHCPh2)(PPh3)3 complex was also obtained and a geometry in solution was proposed.

Graphical abstractThe synthesis of a series of mono and bis(benzophenone imine) complexes of Mn, Re, Ru, and Os is presented. The unprecedented imine complexes of iridium were also prepared by substituting chloride ligand in appropriate precursors.Figure optionsDownload full-size imageDownload as PowerPoint slide