| Summary: | In the present work, using a sonochemical method, a new lead (II) coordination 1D polymer, [Pb(L)<sub>2</sub>(CH<sub>3</sub>COO)]<sub>n</sub> (L = pyridine-4-carbaldehyde thiosemicarbazone) (<b>1</b>) was prepared. It was characterized structurally with different spectroscopic methods, such as SEM, IR spectroscopy, XRD, and elemental analysis. The coordination compound becomes a stair-step one-dimensional polymer in solid mode. The lead (II) ions have the coordination number of six (PbNS<sub>3</sub>O<sub>2</sub>) with two oxygen atoms from acetate anion and three sulfur atoms and one nitrogen atom from organic ligand. It contains a stereo-chemically active lone electron pair and the hemidirected coordination sphere. The high-intensity ultrasound is considered a flexible, environmentally friendly, and easy synthetic tool for the coordination compounds. PbO clusters was achieved with thermolyzing <b>1</b> at 180 ˚C with oleic acid (as a surfactant). Furthermore, the size and morphology of the created PbO clusters were assessed via SEM. The estimated gap of HOMO and LUMO is 3.275 eV based on DFT calculations.
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