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Nickel bis(hydrogen pyridine-2,6-dicarboxylate) trihydrate, Ni(HDP)z.3H20, crystallizes in the monoclinic system, space group P21/c, with a=14.76+0.10, b= 10.05+0.02, c=13.76+0.08 ~, ,/3= 122.2+0.4 °, Z=4. The structure was determined by means of the Patterson function and Fourier syntheses which were calculated from intensities collected on Weissenberg equi-inclination photographs using Cu Ko~ radiation. Prior to the structure refinement, the atoms were divided into two blocks, and anisotropic full-matrix least-squares calculations were successively applied to each (R= 0.087). The Ni atom is surrounded by an unsymmetrical arrangement of the two nitrogen atoms and also four oxygen atoms, each of which belongs to a different carboxylic or carboxylato group. The chelate molecule is thus formed of two orthogonal HDP planes, and the three water molecules are in interstitial positions.