A series of novel complexes with 5-sulphadiazineazo-3-phenyl-2-thioxo-4-thiazolidinone (H2L1) and 5-sulphamethazineazo-3-phenyl-2-thioxo-4-thiazolidinone (H2L2) and various anions were prepared. Their structures and properties were characterized by elemental analyses, IR, UV-vis, EPR spectroscopy and magnetic measurements. The visible and EPR spectral studies indicated that the Cu(II) complexes have distorted octahedral. From the electron paramagnetic resonance and spectral data, the orbital reduction factors k(parallel to) and k(perpendicular to) were calculated. In all cases k(perpendicular to) > k(parallel to) indicates a B-2(1g) ground state. The crystal field parameters for Co(II) and Ni(II) complexes were calculated. The electronic absorption and a g(parallel to)/A(parallel to) values are indicative for the beginning of tetragonal distortion. The complexes, however, have lower symmetries and the amount of distortion in terms of DT/Dp, applying NSH 'Hamiltonian Theory' has been evaluated which indicate that the complexes are moderately distorted. (C) 2001 Elsevier Science B.V. All rights reserved.