A new one-dimensional fluorinated nickel phosphate Ni (HP2O7)F .C2N2H10 has been synthesized solvothermally using ethylenediamine as the template and its structure was determined by means of single-crystal X-ray diffraction, The title compound crystallizes in the monoclinic system, space group C/2c (No. 15) with M = 314.78, a 12.658(3) Angstrom, b = 14.502 (3) Angstrom, c = 10.820(3) Angstrom, beta = 109.924(5)degrees, V = 1867.3(8) Angstrom (3), Z = 8, R = 0.0318, and wR = 0.0670, The structure consists of infinite chains of cis. trans-corner-sharing NiO4F2 octahedra with the adjacent octahedra being bridged by HP2O7 groups, which are H-bonded with amine groups of the organic cations. The Ni-F bond lengths along the backbone of the chain are alternately short and long. The as-synthesized product is characterized by powder X-ray diffraction, IR spectroscopy, inductive couple plasma analysis, thermogravimetric analysis, and differential thermal analysis. (C) 2001 Academic Press.