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Synthesis and solid state characterization of two insoluble tetrathiometalates

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Abstract

The aqueous reaction of ammonium tetrathiometalates (NH4)2[MS4] (M = Mo or W) with (dbtmen)Br2 · 2H2O (dbtmen = N,N′-dibenzyl-N,N,N ′, N′-tetramethylethylenediammonium dication) results in the formation of the highly insoluble compounds (dbtmen)[MoS4] (1) and (dbtmen)[WS4] (2) in near quantitative yields. Compounds (1) and (2) have been characterized by elemental analysis, spectroscopic methods, X-ray powder diffraction and TG–DTA. Both compounds exhibit nearly identical IR spectra and X-ray powder patterns. The compounds exhibit a single strong signal for the asymmetric M–S stretching vibration at 475 cm−1 in (1) and at 457 cm−1 in (2). Complex (2) is thermally more stable than the corresponding Mo analogue (1). Thermal decomposition products of (1) and (2) are carbon contaminated amorphous metal disulfides and are formulated as MoS1.99C2.06N0.07 and WS1.75C3.02 based on elemental analysis of the residue.

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References

  1. A. Müller, E. Diemann, R. Jostes and H. Bögge, Angew. Chem. Int. Ed. Engl., 20, 934 (1981) and references therein

    Article  Google Scholar 

  2. Coucouvanis D. (1998). Adv. Inorg. Chem. 45: 1

    Article  CAS  Google Scholar 

  3. Shibhahara T. (1993). Coord. Chem. Rev. 123: 73

    Article  Google Scholar 

  4. Skrabalak S.E. and Suslick K.S. (2005). J. Am. Chem. Soc. 127: 9990

    Article  CAS  Google Scholar 

  5. Tenne R., Homyonfer M. and Feldman Y. (1998). Chem. Mater. 10: 3225

    Article  CAS  Google Scholar 

  6. Bonneau P.R. and Kaner R.B. (1992). Inorg. Chem. 31: 2127

    Article  CAS  Google Scholar 

  7. Close M.R., Petersen J.L. and Kugler E.L. (1999). Inorg. Chem. 38: 1535

    Article  CAS  Google Scholar 

  8. Afanasiev P., Xia G.F., Berhault G., Jouguet B. and Lacroix M. (1999). Chem. Mater. 11: 3216

    Article  CAS  Google Scholar 

  9. Bezverkhy I., Afanasiev P. and Lacroix M. (2000). Inorg. Chem. 39: 5416

    Article  CAS  Google Scholar 

  10. Li Y.D., Li X.L., He R.R., Zhu J. and Deng Z.X. (2002). J. Am. Chem. Soc. 124: 1411

    Article  CAS  Google Scholar 

  11. Poisot M., Bensch W., Fuentes S. and Alonso G. (2006). Thermochim. Acta 444: 35

    Article  CAS  Google Scholar 

  12. Srinivasan B.R., Vernekar B.K. and Nagarajan K. (2001). Indian J. Chem. 40A: 563

    CAS  Google Scholar 

  13. Srinivasan B.R., Dhuri S.N., Näther C. and Bensch W. (2002). Acta Cryst. E58: m622

    CAS  Google Scholar 

  14. Srinivasan B.R., Dhuri S.N., Näther C. and Bensch W. (2005). Inorg. Chim. Acta 358: 279

    Article  CAS  Google Scholar 

  15. Srinivasan B.R., Dhuri S.N., Näther C. and Bensch W. (2003). Acta Cryst. C59: m124

    CAS  Google Scholar 

  16. Srinivasan B.R., Dhuri S.N., Poisot M., Näther C. and Bensch W. (2004). Z. Naturforsch 59: 1083

    CAS  Google Scholar 

  17. Srinivasan B.R., Dhuri S.N., Poisot M., Näther C. and Bensch W. (2005). Z. Anorg. Allg. Chem. 631: 1087

    Article  CAS  Google Scholar 

  18. Srinivasan B.R., Dhuri S.N., Näther C. and Bensch W. (2006). Monats. Chem. 137: 397

    Article  CAS  Google Scholar 

  19. B.R. Srinivasan, S.N. Dhuri, C. Näther and W. Bensch, Polyhedron (2006) DOI: 10.1016/j.poly.2006.05.039

  20. Srinivasan B.R., Näther C. and Bensch W. (2005). Acta Cryst. E61: m2454

    CAS  Google Scholar 

  21. Srinivasan B.R., Näther C. and Bensch W. (2006). Acta Cryst. C62: m98

    CAS  Google Scholar 

  22. Srinivasan B.R., Dhuri S.N., Näther C. and Bensch W. (2003). Acta Cryst. E59: m681

    CAS  Google Scholar 

  23. Srinivasan B.R., Poisot M., Näther C. and Bensch W. (2004). Acta Cryst. E60: i136

    CAS  Google Scholar 

  24. Srinivasan B.R., Näther C., Naik A.R. and Bensch W. (2006). Acta Cryst. E62: m1635

    CAS  Google Scholar 

  25. Srinivasan B.R., Dhuri S.N. and Naik A.R. (2004). Tetrahedron Lett. 45: 2247

    Article  CAS  Google Scholar 

  26. Desiraju G.R. and Steiner T. (1999). The Weak Hydrogen Bond in Structural Chemistry and Biology. Oxford University Press, Oxford

    Google Scholar 

  27. Wennmohs F., Staemmler V. and Schindler M. (2003). J. Chem. Phys. 119: 3208

    Article  CAS  Google Scholar 

  28. Siemeling U., Bretthauer F. and Bruhn C. (2006). Z. Anorg. Allg. Chem. 632: 1027

    Article  CAS  Google Scholar 

  29. McDonald J.W., Friesen G.D., Rosenhein L.D. and Newton W.E. (1983). Inorg. Chim. Acta 72: 205

    Article  CAS  Google Scholar 

  30. Srinivasan B.R., Dhuri S.N., Sawant J.V., Näther C. and Bensch W. (2006). J. Chem. Sci. 118: 211

    CAS  Google Scholar 

  31. Wolff T.E., Berg J.M., Hodgson K.O., Frankel R.B. and Holm R.H. (1979). J. Am. Chem. Soc. 101: 4140

    Article  CAS  Google Scholar 

  32. Alonso G., Aguirre G., Rivero I.A. and Fuentes S. (1998). Inorg. Chim. Acta 274: 108

    Article  CAS  Google Scholar 

  33. Nakamoto K. (1986). Infrared and Raman Spectra of Inorganic and Coordination Compounds. John Wiley, New York, 130

    Google Scholar 

  34. Ellermeier J., Näther C. and Bensch W. (1999). Acta Cryst. C55: 501

    CAS  Google Scholar 

  35. Ellermeier J., Näther C. and Bensch W. (1999). Acta Cryst. C55: 1748

    CAS  Google Scholar 

  36. Ellermeier J. and Bensch W. (2001). Z. Naturforsch. 56b: 611

    Google Scholar 

  37. Ellermeier J. and Bensch W. (2002). Monatsh. Chem. 133: 945

    CAS  Google Scholar 

  38. Ellermeier J., Stähler R. and Bensch W. (2002). Acta Cryst. C58: m70

    CAS  Google Scholar 

  39. J. Ellermeier, Ph.D. thesis, Christian-Albrecht Universität-Kiel (2002)

  40. Poisot M., Nather C. and Bensch W. (2006). Acta Cryst. E62: m1326

    CAS  Google Scholar 

  41. Alonso G., Saidati M.H., Berhault G., Aguilar A., Fuentes S. and Chianelli R.R. (2004). App. Catal. 263: 109

    Article  CAS  Google Scholar 

  42. Alonso G., Berhault B., Aguilar A., Collins V., Ornelas C., Fuentes S. and Chianelli R.R. (2002). J. Catal. 208: 359

    Article  CAS  Google Scholar 

  43. Prasad T.P., Diemann E. and Müller A. (1973). J. Inorg. Nucl. Chem. 35: 1895

    Article  CAS  Google Scholar 

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Authors and Affiliations

  1. Department of Chemistry, Goa University PO, Goa, 403 206, India

    Bikshandarkoil R. Srinivasan & Sunder N. Dhuri

  2. Institut für Anorganische Chemie, Christian-Albrechts-Universität Kiel, Olshausenstraße 40, D-24098, Kiel, Germany

    Christian Näther & Wolfgang Bensch

Authors
  1. Bikshandarkoil R. Srinivasan
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  2. Sunder N. Dhuri
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  3. Christian Näther
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  4. Wolfgang Bensch
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Correspondence to Wolfgang Bensch.

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Srinivasan, B.R., Dhuri, S.N., Näther, C. et al. Synthesis and solid state characterization of two insoluble tetrathiometalates. Transition Met Chem 32, 64–69 (2007). https://doi.org/10.1007/s11243-006-0126-x

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  • DOI: https://doi.org/10.1007/s11243-006-0126-x

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