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)[enH(2)](2)[Zr-3(OH)(6)(PO4)(4)], the structural control effect of organic solvents were further clarified. (C) 2004 Elsevier B.V. All rights reserved.