Pyrimidyl-2-selenolates of cadmium and mercury: Synthesis, characterization, structures and their conversion to metal selenide nano-particles
作者:Rakesh K. Sharma、Amey Wadawale、G. Kedarnath、B. Vishwanadh、Vimal K. Jain
DOI:10.1016/j.ica.2013.11.018
日期:2014.2
Reactions of [MCl2(tmeda)] (M = Cd or Hg; tmeda = N, N, N', N'-tetramethylethylenediamine) with NaSeC4H(R-4,6)(2)N-2 (R = H or Me) gave selenolate complexes of the general formula [MSeC4H(R-4,6) 2N2} 2 (tmeda) n] (M/R/n = Cd/H/1 (1); Cd/Me/1 (2); Hg/H/1 (3) and Hg/Me/0 (4)). The chloro complexes of general formula, [MClSeC4H(Me-4,6)(2)N-2}(tmeda)] (M = Cd (6) or Hg (7)) have been synthesized by redistribution reaction of [MSeC4H(Me-4,6)(2)N-2}(2)] with MCl2 followed by treatment with tmeda. The complexes have been characterized by elemental analysis, UV-Vis and NMR (H-1, C-13, Se-77, Cd-113 and Hg-199) spectroscopy. The molecular structures of [CdSeC4H(Me-4,6)(2)N-2}(2)(tmeda)] and [HgSeC4H(Me-4,6)(2)N-2}(2)] were established by single crystal X-ray diffraction. The complex, [CdSeC4H(Me-4,6)(2)N-2} 2(tmeda)] comprises of an octahedral cadmium atom containing chelating, two SeC4H(4,6-Me) N-2 and one tmeda, ligands. The complex, [HgSeC4H(Me-4,6) 2N2} 2] has a linear structure with monodentate selenolate ligand. Thermolysis of [CdSeC4H(Me-4,6)(2)N-2}(2)(tmeda)] and [HgSeC4H(Me-4,6)(2)N-2}(2)] in various coordinating solvents afforded CdSe and HgSe nanoparticles which were characterized by UV-Vis, XRD, SEM, EDX and TEM. (C) 2013 Elsevier B.V. All rights reserved.