A series of poly(N-vinyl-2-pyrrolidone-co-N-isopropylacrylamide)s, poly(VP-co-NIPA) copolymers with different compositions were prepared by radical copolymerization of VP and NIPA in N,N'-dimethylformamide at 65 degrees C using 2,2'-azobisisobutyronitrile as initiator. Cu(II)-copolymer macrocomplexes were prepared by complexation of the copolymers with copper sulfate in aqueous solution at 40 degrees C. The structure and composition of the copolymers, and the formation of coordinated Cu(H)complexes between amide VP units and Cu2+ ions, were studied by FTIR spectroscopy, DSC and TGA-DTG in addition to electrical conductivity. Studies on the relationship between composition and thermal behavior showed that the values of T-g and T-d of the copolymers and their coordinated macrocomplexes increased with increasing VP content. The copolymers predominantly show amorphous structure while their Cu(II)-macrocomplexes show the presence of a crystalline phase. The conductive properties of the synthesized Cu(II)-poly(VP-co-NIPA) complexes are also discussed. (C) 2008 Wiley Periodicals, Inc.