Polymeric copper(II) and nickel(II) complexes of a binucleating tetraoxime macrocycle, 6,6'-methylenebis[1,12-di(hydroximino)-2,3;9,10-dibenzo-1,11-diaza-4,8-dithiacyclotridecane] (H4L), have been prepared and characterised by elemental analysis, magnetic moments, i.r., uv/vis., and e.p.r. spectral studies. I.r. spectra show that the ligand acts in a tetradentate manner and coordinates via N, S and O donor atoms. The geometry of the resulting metal chelates is discussed with the help of magnetic and spectroscopic measurements. The elemental analyses, stoichiometry and the spectroscopic data of the complexes indicate that the copper(II) and nickel(II) ions are coordinated by the coordination environment of the ligand. The spectral data suggest a distorted tetragonal geometry for polymeric copper(II), and nickel(II) ions in the complexes. The stoichiometry of the metal-to-H4L ratio of complexes (2) and (3), prepared from CuCl2 and NiCl2 respectively, was 3:1, suggesting the formation of polymeric species.