A novel family of chelating bis-bidentate azodye compounds1with 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,1H and13C NMR, EPR and electronic spectral studies. Tentative structures for the polymeric complexes are proposed. The important IR bands and the main1H and13C signals are assigned and discussed relative to the molecular structure. Various EPR parameters for Cμ(II), have been calculated. The ligand acts as a dibasic bis-bidentate 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 the 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.