A new nano-structured lead(II) coordination polymer, [Pb(mu-bpp)(mu-Br)(2)](n) (PBB) [bpp = 1,3-di(4-pyridyl)propane], has been synthesized by the reaction of a mixture lead(II) acetate and KBr with bpp by both hydrothermal and sonochemical methods. 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 calcination of the nano-structured PBB at vacuum and air atmosphere. The structure of PBB 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 PBB was studied and compared with each other. (C) 2009 Elsevier B.V. All rights reserved.