Synthesis and Structural Characterization of New Lead(II) Discrete and Infinite Cage-Like Framework: A Precursor to Produce Pure Phase Nano-Sized Lead(II) Oxide

A novel Pb(II) complex, {[Pb2(tpmba)2(NO3)4]·MeOH}n (1), was obtained by the reaction of a tripodal ligand, N,N′,N″-tris(pyrid-3-ylmethyl)-1,3,5-benzenetricarboxamide (tpmba), with Pb(NO3)2. The structure of complex was determined by X-ray crystallography. The results of structural analysis of the complex reveal that 1 is a M2L2 cage-like with a methanol molecule beside the cage. An entirely different structure and topology between 1 and similar complexes indicate that the nature of organic ligands affects the structure of assemblies. The results indicate that the framework of this complex is predominated by the nature of the organic ligand, anions, solvent and geometric need of the metal ions. It was found that the coordination number of PbII ions is eight, (PbN3O5) has a stereo-chemically active electron lone pair and the coordination sphere is hemi-directed. PbO nanoparticles are obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant. Scanning electron microscopy shows that the size of the PbO particles is ~30 nm.