Nano-structures of two new Pb(II) three-dimensional coordination polymers, [Pb-2(4-pyc)(2)I-2(H2O)](n) (1), {4-Hpyc = 4-pyridinecarboxilic acid} and [Pb(3-pyc)I](n) (2), {3-Hpyc = 3-pyridinecarboxilic acid} were synthesized by sonochemical method. The new nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compounds 1 and 2 were structurally characterized by single crystal X-ray diffraction and are three-dimensional coordination polymers. The thermal stability of compounds 1 and 2 both their bulk and nano-size were Studied by thermal gravimetric and differential thermal analyses and compared. PbO block-structures were obtained by calcination of the nano-structures of compounds 1 and 2 at 400 degrees C. (C) 2009 Elsevier Ltd. All rights reserved.