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The Cu(II) coordination polymer, [Cu(dpa)(N₃)₂]n (1), has been synthesized by the reaction of 2,2'-dipyridylamine (dpa) and a mixture of Cu(ClO₄)₂·6H₂O and sodium azide under ultrasonic irradiation. The products were characterized by infrared (FT-IR) spectroscopy, X-ray powder diffraction, and scanning electron microscopy (SEM). The CuO nano particles were prepared from calcination of compound 1 at 873 K. The CuO nanoparticles were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM). This study demonstrates that sonochemistry is a suitable method for the preparation of coordination polymer nano-structures and that the calcination temperature can be an effective parameter to control the size of CuO nano-structures prepared by direct calcination of a coordination polymer.

Source of materialTo a solution of pyridine-2-carbaldehyde thiosemicarbazone ligand in methanol (10 ml) was added a aqueous solution of zinc nitrate and excess of sodium Perchlorate. The reaction mixture was stirred for 10 h at room temperature and left in room temperature for five days. The yellow crystals were filtered off, washed with cold methanol and ether and dried in vacuum over P4O10 (mp 488 K; yield 60%). Elemental analyses were consistent with the stiochiometry C7H9CIN4O4S. Melting points were measured on an Electrothermal 9100 apparatus and are uncorrected. DiscussionThe ligand of pyridine-2-carbaldehyde thiosemicarbazone possess a wide range of biological activity depending on the parent aldehyde or ketone. Heterocyclic thiosemicarbazones are important because of their possible beneficial biological activity. In the last twenty years, the metal complexes derived from this ligand have drawn some attention. In most of cases, the ligand is tridentate binding to the metal through the N-pyridine, N-azomethine and S atoms. The chemistry of complexes of this ligand markedly depends on the kind of transition metal ions. In the course of our studies of the syntheses and reactions of amidic and thioamidic derivatives ligands with zinc(II) salts [1,2], we have isolated an interesting adduct of pyridine-2-carbaldehyde thiosemicarbazone and perchloric acid. The adduct structurally characterized by X-ray crystallography.

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