Functionalization of polyoxometalates: From Lindqvist to Keggin derivatives. 1. Synthesis, solution studies, and spectroscopic and ESI mass spectrometry characterization of the rhenium phenylimido tungstophosphate [PW11O39{ReNC6H5}](4-)

Dablemont C; Proust A; Thouvenot R; Afonso C; Fournier F; Tabet JC

Inorganic Chemistry, Vol.43, No.11, 3514-3520, 2004

Dablemont C, Proust A, Thouvenot R, Afonso C, Fournier F, Tabet JC

Reaction of [Bu4N](4)[H3PW11O39] with [Re(NPh)Cl-3(PPh3)(2)], in acetonitrile and in the presence of NEt3, provided the first Keggin-type organoimido derivative [Bu4N](4)[PW11O39{ReNPh}] (Ph = C6H5) (1). The functionalization was clearly demonstrated by various techniques including H-1 and N-14 NMR, electrochemistry, and ESI mass spectrometry. Conditions for the formation of 1 are also discussed.