Development of components that can form large molecular aggregates through non–covalent interactions, in nano size structures, has been an active area of research. In current study, a nano-sized Pb(II) coordination polymer, {[Pb(pydc)(pydc.H₂)(H₂O)₂]₂}_n (1), where [pydc.H₂= 2,6-pyridinedicarboxylic acid), were synthesized by sonochemical method and characterized by field emission scanning electron microscope (FESEM), X-ray powder diffraction (XRD), FT-IR spectroscopy and elemental analyses. The sizes of the nano-structures were approximately 90 nm. The thermal stability of compound 1 has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA). The crystal structure of compound 1, based on an X-ray structural analysis has been reported before, in which the crystal dimensions was in millimeter range. Pure phase PbO nanoparticles were simply obtained by calcination of nano-sized compound 1 at 600 ^°C under argon atmosphere and the particles size of the PbO were about 26 nm. This study demonstrates that the coordination polymers may be suitable precursors for the simple one-pot preparation of nanoscale metal oxide materials with different and interesting morphologies.