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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