Because of the variable valence of Mo,the challenging research field of polyoxomolybdate possesses extended diverse structures.[1,2] A series of Strandberg-type polyanion [(RP)2Mo5O21]4- have been reported by Pope et al in 1975.[3] In this report,a new derivate of polyoxomolybdate Na7H[Ni{Mo2O6CH3C(O)(PO3)2}2]·28H2O(1)was synthesized and reported,which was characterized by X-ray powder diffraction,IR and UV spectra and single-crystal X-ray diffraction.