The self-assembly of 1,10-phenanthroline (phen) and 1,3-benzenedicarboxylic acid (H(2)bdc) with Pb(NO3)(2) under solvothermal conditions in N,N-dimethylacetamide (DMA) gives rise to a one-dimensional chain coordination polymer, [Pb(phen)(bdc)] (1), which was characterized by elemental analysis, FT-IR and single-crystal X-ray diffraction. This complex crystallizes in triclinic, space group P(1) over bar with a = 7.5595(6), b = 9.8199(8), c = 13.1663(11) angstrom, alpha = 69.7590(10), beta = 80.6000(10), gamma = 71.3180(10)degrees, Z = 2, C20H12N2O4Pb, M-r = 551.51, D-c = 2.112 g/cm(3), F(000) = 520 and mu = 9.757 mm(-1). The final R = 0.0304 and wR = 0.0763 for 3427 observed reflections with I > 2 sigma(I) and R = 0.0365 and wR = 0.0894 for all data. The structure contains one crystallographic unique Pb(II) atom, one phen molecule chelating with a Pb(II) atom, and one bdc(2-) anion, acting as bidentate bridging ligand linking the Pb(II) atoms to form a one-dimensional structure. The two-dimensional layer and three.-dimensional stacking structures are formed by C-H center dot center dot center dot O hydrogen bonding interactions. The thermal stable and fluorescent properties of 1 were investigated. PbO micro-crystal particles are produced by calcination of powder sample of complex 1. The obtained PbO is characterized and observed by XRD and SEM analyses.