A new lead(II) coordination polymer, [PbBr 2 (C 9 H 15 N 5 O)] n (1), where C 9 H 15 N 5 O is (2,4-diamino-6-piperidine-1-yl) pyrimidine N-oxide (minoxidil) is synthesized and characterized. Polymer 1 is synthesized in methanol by sonochemical and hydrothermal methods from lead(II) acetate, KBr and the minoxidil ligand. The crystal structure of [PbBr 2 (C 9 H 15 N 5 O)] n indicates a syndiotactic coordination polymer. The Pb(II) atom lies on a mirror plane; the mirror plane is perpendicular to the pyrimidine ring bisecting the piperidine ring. N-HÁÁÁO intramolecular and C-HÁÁÁBr, N-HÁÁÁN strong intermolecular interactions were observed. Micro-rods of PbO and nano-plates of PbOHBr were prepared by thermal decomposition of the nano-structured [PbBr 2 (C 9 H 15 N 5 O)] n as a precursor. Characterization of the products was carried out using X-ray crystallography, elemental analysis, FTIR spectroscopy, scanning electron microscopy, energy dispersive X-ray analysis and thermal analysis. The sonochemical method resulted in a significant reduction of reaction time, reaction temperature and particle sizes of the products.