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Hydrothermal reactions of Na2 Mo O2·2H2O and NH4VO3(or V2O5) with appropriate reducing agents such as organic amines, NH2OH·HCl and Mo(CO)6 gave rise to the formation of a series of capped Keggin derivatives, [N(CH3)4]2Na3(NH4)2[(VVO4)MoVI8VIV4O