Nanoparticles of a three-dimensional supramolecular Cd(II) compound, [Cd(L)(2)(H2O)(2)] (1), (L- = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 in both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared with each other. Concentration of initial reagents effects on size and morphology of nano-structured compound 1, have been studied. Calcination of the single crystals and nano-sized compound 1 at 650 degrees C under air atmosphere yields CdO nanoparticles. (C) 2012 Elsevier B.V. All rights reserved.