Nano-structures of two new Pb(II) coordination polymers, [Pb(DPAcO)2] n (1) and [Pb(MPAcO)2] n (2), HDPAcO=diphenyl acetic acid and HMPAcO=monophenyl acetic acid} were synthesized by a sonochemical method. The new nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compound 2 was structurally characterized by single crystal X-ray diffraction. The crystal structure of the compound 2 consists of one-dimensional polymeric units of [Pb(MPAcO)2] and shows the coordination number in the PbII ions is six. The thermal stability of compounds 1 and 2 were studied by thermal gravimetric and differential thermal analyses and shows that nanostructures of compounds 1–2 are somewhat less stable then their bulk materials. PbO nano-powders were obtained by calcinations of the nano-structures of compounds 1 and 2 at 400°C.