A number of experimental techniques were used to study the changes in the atomic structure of copper(II) acetate-bipyridine under thermal decomposition between 25A degrees C and 700A degrees C to form copper-containing nanoparticles. The dynamics of structural changes during decomposition in a thermogravimetric chamber is compared with X-ray absorption spectra, IR spectra, and diffraction patterns for a sequence of annealing temperatures. The experimental results were used to construct theoretical structural models of the complex under thermal decomposition.