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The reaction of Ni(CH3COO)2·4H2O, Na2MoO4·H2O, MoO3, 1,10-phenanthroline and 1,4-butylenediphosphonic acid in distilled water at 180 ℃ for 72 h produced two new comand 2 both feature {MonO3nO3P(CH2)4PO3}4- (n = 5, 6) 1-D anionic chain, which is further decorated and charge compensated by [Ni(1, 10-phen)2]2+. 1 contains {Mo6O24P2 } cluster constructed of three pairs of face-sharing {MoO6} octahedra linked through corner-sharing interaction. 2 exhibits the characteristic structure based on pentanuclear ring of corner- and edge-sharing{MoO6}octahedra capped by three oxygen atoms of { PO3 } on each side. The therrnogravimetric analyses and magnetic property of 2 were also studied.