New nanostructure lead(II) coordination polymer, [Pb(mu-bdabpm)(mu-Br)(2)](n) [bdabpm=1,4-Benzenediamine, N,N'-bis(3-pyridinylmethylene)], has been synthesized by the reaction of a mixture lead(II) nitrate and KBr with bdabpm by sonochemical method. Reaction conditions, such as temperature, time, concentration and initial reagents play important roles in the size, morphology and crystal growth of the final products. The nano-sized PbBr2 and PbO were prepared from the calcinations of the nanopowders (ncp) at vacuum and air atmosphere. The structure of the compound (ncp, NCP = Nano Coordination Polymer) was determined by X-ray crystallography, while nano-structural materials were characterized by X-ray powder diffraction (XRPD) and Scanning Electron Microscopy (SEM). Thermal stability of bulk and nano-sized particles of ncp was studied and compared with each other. (C) 2012 Elsevier B.V. All rights reserved.