Novel polymeric azomethines of 5,5'-methylene-bissalicylaldehyde with two siloxane diamines {H2N(CH2)(3)(CH3)(2)SiO[(CH3)(2)SiO](m)Si(CH3)(2)(CH2)(3)NH2, where m = 0 or 6.5} were obtained. Their structures were confirmed by elemental and spectral [IR, ultraviolet-visible (UV-vis), and H-1 NMR] analysis. The obtained polyazomethines were converted into the chelates of some divalent metals (copper, cobalt, and nickel). The resulting complexes were characterized by electronic and IR spectral measurements, elemental analysis, and thermal studies. From IR and UV-vis studies, the phenolic oxygen and imine nitrogen of the ligand were found to be the coordination sites. The thermogravimetric data indicated that the chelates were less stable than the corresponding ligands and that the thermostability depended on the siloxane segment length and the nature of the metal. Both the macromolecular ligands and the parts of the resultant chelates were soluble in common organic solvents, such as CHCl3, CH,Cl,, dimethylformamide, and dimethyl sulfoxide. The surface compositions of the ligands and some chelates were examined by X-ray photoelectron spectroscopy. (C) 2003 Wiley Periodicals, Inc.