A (1+1) macrocyclic calix[4]arene based Schiff base derivative has been synthesized and was subjected to complexation with different ions or ionic species, viz., VO2+, UO22 +, Fe3+, Ni2+, Cu2+ and Zn2+. 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 VO2+ and UO22 + 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. © 2009 Elsevier Ltd. All rights reserved.