A new macromolecule ligand and its mixed-valent Cu(I, II) and Fe(II, III) complexes have been prepared by using ethylenediamine as core and maleic anhydride as branched units and characterized by UV-vis, FT-IR, thermal analysis and X-ray photoelectron spectroscopy (XPS). The data obtained from these studies suggested that the coordinate bonds of N-->M, Cl-->M, Ph-OH-->M and H(2)O-->M have been formed and possible binding models are proposed for these complexes. The thermal analysis (TG-DTG) reveals that these complexes possess thermal stable property below 800 degrees C.