Some triple resonance experiments in solid-state CP MAS NMR:: 51V/29Si, 31P/13C, and 29Si/13C

It is shown that the phenylphosphinic acid C6H5PH(O)(OH) and the octavinylsilsequioxane [SiO1.5(C2H2)](8) act as good candidates for the set-up of the Hartmann-Hahn condition under MAS condition for P-31 --> C-13 and Si-29 --> C-13 CP transfer, respectively. The study of the polyoxometalate derivative [AsW9O33('BuSiO)(3)(VO)]((Bu4N)-Bu-n)(3) allowed us to clearly demonstrate the effect of {V-51} decoupling during Si-29 acquisition for this type of compounds. These examples open new possibilities for the detailed study of inorganic compounds and hybrid materials, by triple resonance solid-state NMR experiments.