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Summary form only given. Nano-structure of a new Pb(II) two-dimensional coordination polymer, [Pb(2pyc)(N3)(H2O)]n (1), 2-Hpyc =2-pyridinecarboxylic 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 1 was structurally characterized by single-crystal X-ray diffraction and consists of two-dimensional polymeric units. The thermal stability of compounds 1 was studied by thermal gravimetric and differential thermal analyses and compared. PbO nanopowders were obtained by calcinations of the nano-structure of compound 1 at 400°C. This study demonstrates the coordination polymers may be suitable precursors for the preparation of nanoscale materials and dependent on their packing they may produce different and interesting morphologies.