Reactions of SbCl3 and BiCl3 with M′Se–C5H3(R-3)N (M′ = Li or Na; R = H or Me) gave homoleptic selenolate complexes of the general formula [M{Se–C5H3(R-3)N}3] (M = Sb or Bi). The complexes were characterized by elemental analysis, UV-vis and NMR (1H, 13C and 77Se) spectroscopy. The single crystal X-ray analysis of [M{Se–C5H3(Me-3)N}3]·nH2O (M/n = Sb/1.5 and Bi/0.5) revealed that the antimony complex adopts a trigonal pyramidal configuration with monodentate selenolate ligands while the bismuth analogue acquires a distorted square pyramidal configuration defined by two chelating and one monodentate selenolate groups. Pyrolysis of [M{Se–C5H3(Me-3)N}3] either in a furnace or in hexadecylamine (HDA) at different temperatures gave a variety of M2Se3 nanostructures. Thin films of metal selenides have also been deposited on glass substrate by aerosol-assisted chemical vapor deposition (AACVD). Both nanostructures and thin films of metal selenides were characterized by UV-vis spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and transmission electron microscopy (TEM).
