Metal-substituted ketenes: first 13C and 31P CP/MAS NMR determinations

Abstract

Cross-polarization, combined with magic-angle spinning, has been employed to obtain high-resolution solid-state 13C and 31P NMR spectra of a series of solid, peculiar ketenes, also known as η 1-ketenyl derivatives, bearing as substituents a PPh 3 moiety and a coordinatively unsaturated Pt(II) fragment. Solid-state NMR data found for trans-[PtCl 2( η 2-C 2H 4){ η 1-C(PPh 3)CO}], trans-[PtCl 2{ η 1-C(PPh 3)CO} 2], Ph 3PCCO, trans-[PtCl 2( η 2-C 2H 4){ η 1-CH(PPh 3)COMe}], trans-[PtCl 2{ η 1-CH(PPh 3)COMe} 2] and Ph 3PCHCOMe, are compared with NMR values obtained in solution. The general utility of the CP/MAS NMR technique in the study of unstable or insoluble complexes is discussed.