Journal of Thermal Analysis and Calorimetry

, Volume 120, Issue 2, pp 1203–1215 | Cite as

Ethane-1,2-dithiolato bridged (μ2) complexes of bis(N,N-diorganodithiocarbamato-S,S′)antimony(III)

Synthesis, characterization and thermal studies
  • Jaswant Carpenter
  • Sapana Joshi
  • H. P. S. Chauhan
Article
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Accepted:

Abstract

Antimony(III) complexes [(Et2NCS2)2Sb-µ2-S(CH2)2SSb(S2CNR2)2] where NR2 = NMe2, N i Pr2, N(CH2CH2)2, N(C6H11)2 and N(CH2CH2)2O 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 (1H and 13C)] 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 °C), and we obtained a semiconducting material, antimony sulfide (Sb2S3), 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.

Keywords

Antimony(III) Dithiocarbamate Thermal analysis Powder XRD Antimony sulfide 
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Notes

Acknowledgements

University Grant Commission (UGC), New Delhi is gratefully acknowledged for providing the research Grant [F.39–801/2010(SR)] for the accomplishment of this work. We are thankful to CSMCRI, Bhavnagar, Gujarat; Sophisticated Analytical Instrumentation Facility (SAIF), Chandigarh, and SAIF, Mumbai for TG/DTA; ESI-Mass and far-IR spectral studies, respectively. The authors thank to IISER, Bhopal, and UGC-DAE-CSR, Indore, for NMR (1H and 13C) and Powder XRD studies, respectively.

Supplementary material

10973_2015_4394_MOESM1_ESM.docx (1.3 mb)
Supplementary material 1 (DOCX 1323 kb)
10973_2015_4394_MOESM2_ESM.docx (12 kb)
Supplementary material 2 (DOCX 11 kb)

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Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2015

Authors and Affiliations

  • Jaswant Carpenter
    • 1
  • Sapana Joshi
    • 1
  • H. P. S. Chauhan
    • 1
  1. 1.School of Chemical SciencesDevi Ahilya UniversityIndoreIndia

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