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The nanorods of [Pb(L)Br₂]_n (1) (L = 1,2-bis (pyridin-3-ylmethylene)hydrazine) underwent ultrasound irradiation and were synthesized as a novel three-dimensional fishbone-like Pb(II)–organic coordination supramolecular compound. The morphology and nanostructure of the synthesized compound were determined through SEM, FTIR, elemental analyses, and XRD. Compound 1 was structurally characterized by single-crystal X-ray diffraction and revealed six-coordinated Pb (II) ions bonded to two N atoms from two L ligands and four bromine anions, forming a one-dimensional fishbone-like coordination polymer, which extended into a 3D supramolecular structure through weak intermolecular interactions. The bulk thermal stability of compound 1 was examined using thermogravimetric analysis (TGA). Moreover, PbO nanoparticles with sizes of 40–80 nm were obtained through the thermolysis of 1 at 180 °C using oleic acid as a surfactant.