A novel one-dimensional chain zirconium phosphate inorganic polymer, [NH4]3[Zr(OH)2(PO4)(HPO4)], has been synthesized in a nonaqueous medium, and characterized by means of single-crystal X-ray diffraction, IR, TG-DTA, ICP and CHN elemental analysis. The needle-like crystals of this compound are formed by macroanionic (empirical formula [ZrP2O10H3]3−) chains of ZrO4(OH)2 octahedra, PO4 and HPO4 tetrahedra, separated by NH4+ cations. By comparing the synthesis condition and crystal structure of the title compound with those of a new layered [NH4]2[enH2]2[Zr3(OH)6(PO4)4], the structural control effect of organic solvents were further clarified.