In the first part of this project , a novel bispyridylamide ligand H 2 bpmb having two coordinating domain, each acting as a bidentate donor, and metaphenylene bridging groups, and the binuclear Co(III), Cu(II) and Ni(II) complexes of its deprotonated form, acting as building blocks for supramolecular architecture have been synthesized and characterized. The crystal structures of these complexes have been determined. by X-ray crystallography. One molecular box with two Cu(II) center and also two binuclear triple stranded helix complexes with Co(III) and Ni(II) have been detected.The number of solvent molecules of compounds have been determined by thermogravimetric analysis (TG) and cyclice voltametry has been used to determine the communication between two metal center and streo and electronic effect in copper and cobalt complexes. In the second part of project a novel less rigid ligand, H 2 mpb, has been synthesized and characterized by IR, Mass and 1H-NMR, X-Ray crystallography. The structural data have been used to rationalize the splitting of the NH peack in the IR spectrum.