Schiff bases play an important role in inorganic chemistry as they easily form stable complexes with most transition metal ions [1]. Transition metal complexes of Schiff base compounds are used as growth inhibiting agents for most of bacteria and fungi [2] also he binding interaction of transition metal complexes with DNA is of interest for both therapeutic and scientific reasons. [3]. In previous works, we reported synthesis and characterization of some macroacyclic Schiff base complexes containing 2-hydroxybenzaldehyde moiety and their antibacterial study [4]. my asymmetrical amine were prepared according to literature method [5]. In this work,many new macroacyclic Schiff base complexes from condensation of asymmetrical amine and O-vaniline and salicylaldehyde in the presence of Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) metal ions were prepared. The complexes were structurally characterized by elemental analyses, IR, UV Vis, NMRand molar conductivity.The crystal structures of tree complexes, [NiL1] (Fig 1), [NiL1] and [ZnL2] have beendeterminedbyasinglecrystalX-raydiffractionstudy.