A novel family of chelating bis-bidenrate azodye compounds(1) with Cu(II), Co(II), Ni(II), Fe(II), Hg(II), Pd(II), UO2(II), Fe(III), Cr(III), La(III), Ru(III)and Zr(IV)has been prepared and characterized on the basis of analytical, magnetic, H-1 and C-13 NMR, EPR and electronic spectral studies. Tentative structures for the polymeric complexes are proposed. The important IR bands and the main H-1 and C-13 signals are assigned and discussed relative to the molecular structure. Various EPR parameters for Cu(II), have been calculated. The ligand acts as a dibasic bis-bidenrate chelating agent coordinating through CO, N=N, COOH and OH groups by replacement of a proton from the two latter groups. Considerable interest has also been focused on thr synthesis of the azo compound and its polymeric metal complex due to its wide potential applications. The thermal decomposition behavior of the complexes is also discussed.