NEW NANOSTRUCTURE LEAD(II) COORDINATION POLYMER, [PB(M-BDABPM)(M-BR)2]N [BDABPM = 1,4- BENZENEDIAMINE, N,N'-BIS(3-PYRIDINYLMETHYLENE)], HAS BEEN SYNTHESIZED BY THE REACTION OF A MIXTURE LEAD (II) NITRATE AND KBR WITH BDABPM BY SONOCHEMICAL METHOD. REACTION CONDITIONS, SUCH AS TEMPERATURE, TIME, CONCENTRATION AND INITIAL REAGENTS PLAY IMPORTANT ROLES IN THE SIZE, MORPHOLOGY AND CRYSTAL GROWTH OF THE FINAL PRODUCTS. THE NANO-SIZED PBBR2 AND PBO WERE PREPARED FROM THE CALCINATIONS OF THE NANOPOWDERS (NCP) AT VACUUM AND AIR ATMOSPHERE. THE STRUCTURE OF THE COMPOUND (NCP, NCP = NANO COORDINATION POLYMER) WAS DETERMINED BY X-RAY CRYSTALLOGRAPHY, WHILE NANO-STRUCTURAL MATERIALS WERE CHARACTERIZED BY X-RAY POWDER DIFFRACTION (XRPD) AND SCANNING ELECTRON MICROSCOPY (SEM). THERMAL STABILITY OF BULK AND NANO-SIZED PARTICLES OF NCP WAS STUDIED AND COMPARED WITH EACH OTHER. THE ELEMENTAL ANALYSIS AND IR SPECTRA OF THE NANOPOWDERS AND OF THE SINGLE CRYSTALLINE MATERIAL ARE INDISTINGUISHABLE. THE ORTEP DIAGRAMS AND PACKING OF THE TITLE COMPLEXES ARE SHOWN IN FIG. 1. COMPOUND (NCP) IS TWODIMENSIONAL NEUTRAL METALLOPOLYMER AND CONSISTS OF THE LEAD (II) IONS BRIDGED BY BOTH BDABPM AND BROMIDE LIGANDS, THUS FORMING A TWO-DIMENSIONAL INFINITE FRAMEWORK [1-4].