A cadmium(II) complex tetrakis(1,3-diazinane-2-thione)cadmium(II) sulfate [Cd(Diaz) 4 ]SO 4 (1) is prepared and its crystal structure is determined by X-ray crystallography. The crystal structure of 1 consists of [Cd(Diaz) 4 ] 2+ and 2 4 SO − ions. In the complex ion, the central cadmium atom is coordinated by four Diaz molecules through sulfur atoms adopting a distorted tetrahedral geometry. The molecular structure is stabilized by N-H…O and N-H…S hydrogen bonding interactions. The complex is also characterized by IR and NMR spectroscopy and the spectroscopic data are discussed in terms of the nature of bonding.In recent years, considerable research efforts have been devoted to the structural characterization of cadmium(II) complexes of thioamides [1-22] because of their applications in biological systems [23,24], in analytical chemistry [25,26], in environmental toxicology [27], and as precursors for the preparation of CdS nanoparticles [28][29][30]. These structural reports describe that in most of the cases, cadmium(II) complexes exist as neutral monomeric [3][4][5][6][7][8][9][10][11][12][13][14][15][16] or polymeric [17][18][19] molecules of the general formula [CdL 2 X 2 ] with the cadmium atom possessing a tetrahedral or distorted octahedral coordination environment respectively. In some cases, ionic complexes of the type [CdL 4 ]X 2 (X = nitrate or sulfonate) are also formed [21, 22]. Recently, we have reported the crystal structures of two new complexes [Cd(Detu) 4 (SO 4 )] (Detu = N,N′diethylthiourea) [1] and [Cd(Diaz) 2 (CH 3 COO) 2 ] (Diaz = 1,3-diazinane-2-thione) [2] in which cadmium(II) shows severe distortions from the octahedral geometry. In view of our continued interest in the structural chemistry of cadmium(II) complexes with thiones [1-10], we report here the synthesis and crystal structure of a cadmium(II) complex of the heterocyclic ligand 1,3-diazinane-2-thione (3,4,5,6-tetrahydropyrimidine) [Cd(Diaz) 4 ]SO 4 . Experimental. Materials. Cadmium sulfate (CdSO 4 ⋅8/3H 2 O) was obtained from Merck Chemical Company, Germany. Diazinane-2-thione (Diaz) was prepared according to the procedure published in the literature [31].Synthesis of [Cd(Diaz) 4 ]SO 4 (1). The title complex was prepared by adding 0.24 g (2.0 mmol) of Diaz in 15 ml of methanol to an aqueous solution (5 ml) of cadmium sulfate (1.0 mmol, 0.26 g) and stirring the mixture for 30 min. The very light yellow cloudy solution was filtered and the filtrate was kept at room temperature for crystallization. As a result, the offwhite crystalline product was obtained, which was washed with methanol and dried.