Co(II) and Cu(II) complex with sulphadiazine have been synthesized and characterized. On the basis of elemental analysis and molar conductance, general formulas Co(C10H10N4O2S)2VO3⋅H2O and Cu(C10H10N4O2S)2VO3⋅H2O have been suggested for the complexes under study. The geometries of the complexes have been proposed on the basis of magnetic moment, electronic and infrared spectral data. Thermo gravimetric analyses(TGA) have been carried out to determine the pattern of their decomposition. The crystal system, lattice parameters, unit cell volume and number of molecules in it have been determined by Xray diffraction data (XRD).