Two novel complexes [Zn(Him-thz)(2)(NO3)](NO3)-N-. 1 and [Ni(Him-thz)(2)(NO3)](NO3)-N-. 2 (Him-thz = 2-(2'-thiazole)-4,4,5,5-teramethyl-dihydro-1H-imidazolyl-l-hydroxy) have been prepared and structurally characterized by X-ray diffraction method. Both complexes crystallize in orthorho- mbic, space group P2(1)2(1)2, Z = 2. Crystal data for 1: ZnC20H30N8O8S2, M-r = 640.2, a = 13.1630(14), b = 10.5149(11), c = 10.6670(11) angstrom, V = 1476.4(3) angstrom(3), D-c = 1.440 g/cm(3), mu(MoK alpha) = 1.028 mm(-1), F(000) = 664, R = 0.0398 and wR 0.0901 for 2131 observed reflections with 1 > 2 sigma(1). Crystal data for 2: NiC20H30N8O8S2, M-r = 633.36, a = 13.1611(7), b = 10.4833(6), c = 10.6928(6) angstrom, V = 1475.30(14) angstrom(3), D-c = 1.426 g/cm(3), mu(MoK alpha) = 0.854 mm(-1), F(000) = 660, R = 0.0281 and wR = 0.0797 for 3099 observed reflections with 1 > 2 sigma(1). X-ray analysis reveals that the crystal structures consist of [M(Him-thz)(2)(NO3)](+) (M = Zn, Ni) moiety and a NO3- anion. Both Zinc(II) and Nickel(II) ions are six-coordinated with distorted octahedral geometries.