A new sonochemical synthesis was utilized to synthesize nanostructures of a novel lead (II) metal-organic coordination polymer, {[Pb2(2-apinh)2(Br)4]}n (1) (2-apinh: 2-acetylpyridine isonicotinoylhydrazone). The effects of reaction time, concentrations, and the irradiation power have been investigated and the optimized synthesis parameters were identified. The compound has been categorized by elemental analysis, scanning electron microscopy (SEM), FT-IR spectroscopy, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) powder X-ray diffraction (PXRD), and single-crystal X-ray analysis.The crystal form of 1 shows two different Pb coordination spheres in the structure, with the crystal taking three-dimensional coordination polymer shape. The coordination numbers of lead (II) centers are seven and eight with holodirected and hemidirected coordination sphere. The adjoining chains are linked by pi-pi interactions of the adjacent aromatic 2-apinh rings and several other relatively weak interactions. These weak interactions further enable the self-assembly of 1 to form a 3D metal-organic coordination polymer.