Ethane-1,2-dithiolato bridged ( mu super(2)) complexes of bis(N,N-diorganodithiocarbamato-S,S')antimony(III)

Antimony(III) complexes [(Et sub(2)NCS sub(2)) sub(2)Sb- mu super(2)-S (CH sub(2)) sub(2)SSb(S sub(2)CNR sub(2)) sub(2)] where NR sub(2) = NMe sub(2), N super( i )Pr sub(2), N(CH sub(2)CH sub(2)) sub(2), N(C sub(6)H sub(11)) sub(2) and N(CH sub(2)CH sub(2)) sub(2)O have been synthesized by the reactions of bis(N,N-diethylthiocarbamato-S,S')antimony(III), ethane-1,2-dithiol and bis(N,N-diorganothiocarbamato-S,S')antimony(III) in 1:1:1 stoichiometries. All the complexes were obtained as yellow solids and are soluble in common organic solvents such as benzene, hexane and chloroform. These complexes have been characterized by molecular weight determination, elemental analyses (C, H, N, S and Sb) and spectral [UV-visible, FT-IR, far-IR, NMR ( super(1)H and super(13)C)] studies. Thermal analysis (TG and DTA) have been applied in inert atmosphere to study the thermal behavior of the complexes. Multi-step decomposition has been observed in the TG curve of the compounds. The results indicate that most of the organic part of the ligands has lost in initial stage of decomposition (40-310 degree C), and we obtained a semiconducting material, antimony sulfide (Sb sub(2)S sub(3)), as a last decomposition product for all the analyzed complexes. Thermal studies in combination with ESI-Mass spectral analysis have provided a comparative insight about the thermal stability of various bis(N,N-diorganodithiocarbamato-S,S')antimony(III) moieties. Powder X-ray diffraction studies provide the information concerning particle size of nanometer range (3.87-10.09 nm) with monoclinic crystal system.