The capability of metal ions to promote the template synthesis of macrocyclic ligands has been studied extensively and depends on several factors related to the ligand characteristics, as well as on the nature of the metal ion [1]. The stability of macrocyclic metal complexes depends upon a number of factors, including the number and type of donor atoms presenting in the ligand and their relative positions within the macrocyclic skeleton, as well as the number and size of the chelate rings formed on complexation. For transition metal ions, features such as the nature and magnitude of crystal-field effects play also an important role [2]. One of the features of non-rigid large ring macrocyclic ligands is their ability to fold to give, have involved the synthesis of ligands with rigid backbones to prevent the folding which can otherwise occur [3-4]. In this work, three new complexes were prepared with direct [1+1] condensation of 2,6-Diformyle-4-phenyle phenol (DFP) and 4,7-bis(2-pyridylmethyl)-4,7-diazadecane-1,10-diamine in methanol followed by addition of Cd(NO3)2.4H2O, MnCl2.2H2O and Zn(ClO4)2.xH2O (Scheme 1). Then the solution was filtered whilst hot and NaClO4 added to the filtrate. The resultant complexes were characterized by IR, Mass, CHN , 1H and 13C NMR spectroscopy. In the IR spectrum, a band at about 1660 cm-1 indicated the formation of C=N bonds, no peaks attributed to NH2 and carbonyl groups implied that the condensation reaction had been completed.