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Reaction of the monosodium salt of (3H-2-thioxo-1,3,4-thiadiazol-2-yl)thioacetic acid, Na(C₂HN₂S₃CH₂COO)∙H₂O (1) with NiSO₄∙7H₂O produced the corresponding nickel(II) complex, Ni(C₂HN₂S₃CH₂COO)₂·nH₂O where n = 4 (2) and 6 (3). The product was characterized by means of microanalysis and thermal analysis. The crystal structure of 3 was determined by single-crystal X-ray diffraction. The molecular structure consists of discrete molecular units: one octahedral [Ni(H₂O)₆]²⁺ cation and two organic anions, (C₂HN₂S₃CH₂COO)^–. The supramolecular structure of 3 is discussed by comparison with that of 1 in its decahydrate, dinuclear form, [Na(C₂HN₂S₃CH₂COO)(H₂O)₄]₂×2H₂O (1’), and reveals the self-assembly of the ionic units into alternating columns through N-H∙∙∙O, O-H∙∙∙O/S and S∙∙∙S interactions.

Keywords: mercapto-1,3,4-thiadiazole derivatives; nickel(II) complex; thermal decomposition; crystal structure.