Preparation of imine complexes of ruthenium and osmium stabilised by [MCl(η 6-p-cymene)(PR3)]+ fragments

Abstract

Imine complexes [MCl(η 6 -p- cymene){η 1 -NH C(H)Ar}(PR 3 )]BPh 4 ( 1 – 3 ) [M = Ru, Os; PR 3 = PPh(OEt) 2 , PPh 2 OEt; Ar = Ph, p- tolyl] were prepared by reacting MCl 2 (η 6 -p- cymene)(PR 3 ) precursors with benzyl azide ArCH 2 N 3 in the presence of NaBPh 4 . Benzophenone-imine complexes [MCl(η 6 -p- cymene){η 1 -NH CPh 2 }(PR 3 )]BPh 4 ( 4 – 6 ) [M = Ru, Os; PR 3 = PPh(OEt) 2 , PPh 2 OEt] were also prepared by allowing MCl 2 (η 6 -p- cymene)(PR 3 ) to react with Ph 2 C NH in the presence of NaBPh 4 . The complexes were characterised spectroscopically (IR, 1 H, 13 C, 31 P, 15 N NMR) and by X-ray crystal structure determination of [RuCl(η 6 -p- cymene){η 1 -NH C(H) -p- tolyl}{PPh(OEt) 2 }]BPh 4 ( 1b ).