Dioximates of Co(III) that contain sulfanilamide have a benefic influence upon the enzymogenesis process of some fungal strains producing exocellular hydrolases with different enzymatic systems. Using the above scheme a new oxime DsamH2 (1) that can be precursor for coordination compounds with biological activity was obtained. The interaction of H2L with CuSO4 resulted in new complex [Cu(DsamH2)3]SO4 .5H2O (2). The structure and composition of 1 and 2 have been characterized using elemental analysis, IR, NMR and X-ray. In the IR spectrum of 1 are observed the bands at ν(NH)=3423, 3357, 3283, ν(C=N)=1642, ν(CC)arom=1592, ν(SO)=1302, 1150, ν(NO)=935 and δ(CH)=767, 725 cm-1 that confirm the condensation of sulfanilamide to dichloroglyoxime. In the 1H NMR spectrum of 1 are present two dublets 7.54 (2H, J=8.78 Hz) and 6.89 ppm (2H, J=8.78 Hz) of the aromatic ring, one signal at 7.16 ppm that belongs to NH2 close to SO2 group, one signal at 8.77 ppm of NH group and one signal at 10.89 ppm of OH group. The sulfanilamide is condensed via NH2 group close to aromatic ring. The signal of this group is higher downfield comparing with the free sulfanilamide and by integration has only one proton. In the 2D HMBC experiment, the protons of NH and OH groups have cross peaks at the shift of oxime carbone, that proves the condensation of sulfanilamide with dicloroglyoxime.figure 1Fig. 1. Structure of DsamH2figure 2Fig. 2. Structure of complex cation [Cu(DsamH2)3]2+A new organic compound 1 crystallizes in the form of yellow prisms, 0.18x0.18x0.12 mm dimensions, in the trigonal space group P3121: a = 8.2460(3), b = 8.2460(3), c = 23.670(2) Å, γ = 120°. Composition C14H16N6O6S2, M = 428.45, Z = 3, T = 293K, Final R value (I>2σ(I)) = 0.0472. The result of X ray study showed that the asymmetric part of the unit cell contains one half of crystallographically independent compound (Fig. 1). The complex 2 crystallizes in the red plates, 0.5x0.3x0.02 mm dimensions, in the monoclinic space group P21/c : a = 15.3330(9), b =14.9758(7), c= 28.788(2) Å, β = 97.794(6)°. Composition C42H58CuN18O27S7, M = 1535.02, Z = 4, T = 293K, Final R value (I>2σ(I)) = 0.0753. The asymmetric part of the unit cell 2 consists of complex cation, inorganic anion and water molecules. Fig. 1 presents the structure of molecule DsamH2 that obeys twofold rotation symmetry, Fig. 2 – the structure of Cu(II) complex cation.