A new series of macrocyclic imine-oxime complexes prepared by template condensation of o-phenylenediamine, phthaldialdehyde, 2,6-diacetylpyridine and dichloroglyoxime in MeOH solution, have been characterized by i.r., electronic spectral data, elemental analyses, conductivity and magnetic susceptibility measurements. In the imine moiety of the complexes, the chloride ions coordinate to the nickel ion. From conductivity measurements, it was shown that the complexes are not all electrolytes. Their thermal behaviour has been studied by the t.g. and d.t.a. analysis. They decompose with loss of the organic ligand and halogen to leave the metal oxide.