The preparation and characterization of metal complexes with macrocyclic or macro-acyclic ligands was the goal of much research in recent years. Bioinorganic chemistry, material science, catalysis, separation and encapsulation processes, hydrometallurgy, formation of compounds with unusual properties, metal-metal interactions, transport and activation of small molecules have received considerable stimulus from the employment of such ligands [1]. Macro-acyclic ligands have been synthesized to verify the influence of the donor atoms and their relative positions, the number and size of the chelate ring formed, the flexibility and the shape of the coordinating moiety, their planar or tridimensional architecture, etc. on the metal ion binding and selectivity. Piperazine is a cyclic diazine with a rigid cyclohex-ane ring and a suitable structural moiety for macrocyclic and macroacyclic compounds [2]. In this work, we report the synthesis and characterization of new macroacyclic Schiff base complexes have been prepared via the Ni(II) or Co(II) or Zn(II) of 2-((4-(2-aminoethyl)-1,4-diazepan-1-yl)methyl)benzenamine with salicylaldehyde.The complexes have been characterized by elemental analysis, IR and 1HNMR.