Laboratory experiment demonstrates oxygen transfer from a molybdenum-trisubstituted tungstophosphate to triphenylphosphine, indicating clean reduction while preserving the core Keggin structure.
The A-type trisubsituted, β-isomer of tetrabutylammonium 3-molybdo-9-tungstophosphate(3-), A-β-[NBun4]3[PMoVI3W9O40], reacted with triphenylphosphine in acetonitrile to afford triphenylphosphine oxide and an oxygen-deficient two-electron reduced species, A-β-[NBun4]3[PMoVIMoV2W9O39]. The reduced species was isolated and characterized by IR, 31P NMR, and X-ray photoelectron spectroscopies. The corner-sharing bridging oxygen atom in a Mo(VI)–O–Mo(VI) skeleton was eliminated upon the reduction, affording two Mo(V) ions in the polyanion moiety retaining the Keggin-type structure.
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Kawafune et al. (1994) studied this question.
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