A novel three-dimensional lead(II) coordination polymer, [Pb-3(dmp)(2)Cl-6] (n) , was prepared by reacting lead(II) chloride with 2,9-dimethyl-1,10-phenanthroline in a fast and facile process. The complex was fully characterized on the basis of its H-1 and C-13 NMR, IR, and UV spectra and elemental and thermal analyses. The molecular structure of the compound was determined by single-crystal X-ray diffraction and its photoluminescence properties were investigated. The single-crystal X-ray data showed that the compound crystallized in the triclinic crystal system in the space group PA << I". The complex was utilized as a precursor for the preparation of PbO nanoparticles by direct thermal decomposition at 600 A degrees C in air. The prepared PbO nanoparticles were characterized by scanning electron microscopy and powder X-ray diffraction and a band gap of ca. 3.76 eV was determined from the UV-Vis absorption spectrum. A strong blue emission, centered at 466 nm, was observed in the photoluminescence spectrum of PbO nanoparticles and that related to oxygen vacancies in PbO.