Synthesis and characterization of organotin(IV) semicarbazones: potential precursors for nanosized tin oxide

Abstract

A series of organotin(IV) semicarbazone adducts of the type R₂SnCl₂·nLH (1–6) were synthesized by the reactions of R₂SnCl₂ with newly synthesized carvone semicarbazone (LH) in anhydrous ethanol [where R = CH₃, n = 1 (1), 2 (2); R = C₄H₉, n = 1 (3), 2 (4); and R = C₆H₅, n = 1 (5), 2 (6)]. All the compounds have been characterized by elemental analyses, FT-IR, NMR (¹H, ¹³C, ¹¹⁹Sn) and FAB mass spectral studies. ¹¹⁹Sn NMR studies suggest monodentate mode of attachment of the ligand with central tin atom in the solution state. Thermogravimetric study of (6) shows large thermal events. Transformations of (4) and (6) to pure tin oxides (i and ii, respectively) have been carried out using sol–gel technique. Powder XRD patterns of the formed tin oxides indicate the formation of tetragonal cassiterite structure. SEM images of (i) and (ii) show wire- and grain-like morphologies of the crystallites, respectively.

Graphical Abstract

A series of organotin(IV) semicarbazone adducts were synthesized by the reactions of diorganotin dichloride with newly synthesized carvone semicarbazone. Transformations of some of the newly synthesized adducts to pure tin oxides have been carried out using sol–gel technique. Powder XRD patterns of the formed tin oxides indicate the formation of tetragonal cassiterite structure, while SEM images show wire- and grain-like morphologies.