Abstract

95Mo solid-state NMR spectra of a variety of molybdates of alkali metals as well as molybdates of some divalent metals, MoO 3, Mo(CO) 6, polyoxo complexes H 3PMo 12O 40·χH 2O and [(C 4H 9) 4N] 4·[Mo 8O 26] are reported. Alkali-metal molybdates show mainly sharp single resonances. Signals from the molybdates of divalent metals show a splitting due to second-order quadrupole effects. For MoO 3, signals from structurally inequivalent Mo sites seem to be resolved. The 95Mo spectrum of H 3PMo 12O 40·χH 2O exhibits a large chemical shift anisotropy, while for [(C 4H 9) 4N] 4·[Mo 8O 26] the superposition of a sharp peak from almost regular MoO 4 tetrahedra and a broad line from Mo atoms in distorted octahedra is observed. For molybdates the resonances are shifted upfield with decreasing MoO bond length. The results can be used for studying molybdenum-based catalysts.

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