In this study the template synthesis and characterization of two new series of Zn(II), Co(II),rnand Cu(II) metal complexes of polyaza macrocyclic ligands are presented.rnIn the first part of this work template condensation reaction of o-phenylenediamine withrnsuccinic acid in a 1:1 molar ratio in the presence of divalent transition metal ions [Zn(II),rnCo(II) and Cu(II)], led to the formation of new series of polycrystalline macrocyclicrncomplexes. The synthesis is a remarkably facile one requiring only stirring under roomrntemperature for short period of time. Elemental analysis shows that the complexes have a 1:1rnligand to metal stoichiometry. The absence of bands characteristic of primary amines andrncarboxylic acids functional groups and the presence of bands characteristic of coordinatedrnsecondary amine in the N-H and M-N region gave a strong evidence for the formation of thernproposed metal complexes. The 1H and the 13C NMR spectra for Zn(II) complex from the firstrnseries also confirm the formation of the macrocyclic frame work. The coordination geometryrnis found to be octahedral for the Zn(II) and Co(II) complexes and square planar for the Co(II)rncomplex.rnIn the second part of the work, template condensation reaction of p-phenylenediamine,rnethyelenediamine, formaldehyde and succinic acid in the presence of metal ions [Zn(II),rnCo(II) and Cu(II)] produced metal complexes of octahedral geometry of bis(macrocycles)rnframework. The formation of such series of complexes was confirmed by physico-chemical studies such as elemental analysis for the metal and chlorine, infrared spectroscopy, electronicrnspectral studies and conductivity data.rnLastly, preliminary investigation on the potential hydrolytic nature of the Zn(II) metalrncomplexes revealed that the complexes possess no significant catalytic nature in thernhydrolysis of p-nitrophenyl phosphate and carboxylate ester. This is probably due to thernpresence of elctrophilic carbonyl carbon site on the macocycles of the complex that competernfor Zn-OH- nucleophile and thereby deactivating its catalytic activity and the formation ofrnpolymeric hydroxide precipitate of the complexes at higher pH.