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

Cross-polarization, combined with magic-angle spinning, has been employed to obtain high-resolution solid-state C-13 and P-31 NMR spectra of a series of solid, peculiar ketenes, also known as eta (1)-ketenyl derivatives, bearing as substituents a PPh3 moiety and a coordinatively unsaturated Pt(II) fragment. Solid-state NMR data found for trans-[PtCl2(eta (2)-C2H4){eta (1)-C(PPh3)Co}], trans-[PtCl2{eta (1) -C(PPh3)CO}(2)], Ph3PC=C=O, trans-[PtCl2(eta (2)-C2H4) {eta (1)-CH(PPh3)COMe}], trans-[PtCl2{eta (1)-CH(PPh3)COMe}(2)] and Ph3PCHCOMe, 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. (C) 2001 Elsevier Science B.V. All rights reserved.