Abstract A (1+1) macrocyclic calixarene based Schiff base derivative has been synthesized and was subjected to complexation with different ions or ionic species, viz., VO 2+, UO 2 2 + , Fe 3+, Ni 2+, Cu 2+ and Zn 2+. Both the conjugate and the complexes were characterized using various spectral techniques, viz.; FTIR, 1H, 13C NMR and FAB mass. The complexes have been further characterized by UV–Vis, EPR and magnetic susceptibility, while the iron complex was studied further by Mössbauer spectroscopy. On the basis of all these studies, the VO 2+ and UO 2 2 + complexes were found to be mononuclear, whereas all the other complexes were found to be dinuclear. Based on the studies, the iron complex was found have a distorted octahedral high spin Fe(III) center with an antiferromagnetically coupled dinuclear core in the complex.