A new nano-sized lead(II) coordination polymer, [Pb(2-bpdh)(NO3)2]n (1); (2-bpdh = 2,5-bis(2-pyridyl)-3,4-diaza-2,4-hexadiene)}, was synthesized by a sonochemical method. The structure of 1 may be considered coordination polymer of lead(II) consist of metallocyclicchains formed by bridging NO3- and 2-bpdh ligands. The thermal stability of compound was studied by thermal gravimetric and differential thermal analyses. The new nano-structure coordination polymer was characterized by scanning electron microscopy, powder X-ray diffraction, elemental analyses and IR spectroscopy. The size of the samples was about 50 nm. Nano-particles of PbO were obtained by thermolysis of compound 1in oleic acid as a surfactant at 180 °C under air atmosphere and the size of this PbO particles were about 50 nm.