Chemical Papers

, Volume 68, Issue 2, pp 210–216 | Cite as

A new organically templated magnesium sulfate: structure, spectroscopic analysis, and thermal behaviour

  • Dhouha ben Hassan
  • Walid RekikEmail author
  • Houcine Naïli
  • Tahar Mhiri
Original Paper


A new magnesium sulfate templated by 2-methylpiperazine, (C5H14N2)[Mg(H2O)6](SO4)2, was prepared by the slow evaporation method. The obtained crystals were investigated by the Raman and FTIR spectroscopy and crystallographically characterised by single-crystal X-ray diffraction. The compound crystallises in the monoclinic system, space group P21/n. Supramolecular network of this hybrid material consists of Mg2+ cations octahedrally coordinated by six water molecules, sulfate tetrahedra and protonated and disordered diamine linked together by two types of hydrogen bonds: OW—H…O and N—H…O. Dehydration of the title compound takes place in three steps. Thermal decomposition of the anhydrous phase consists in the loss of the organic moiety and one sulfate group leading to the formation of magnesium sulfate.


amine magnesium sulfate supramolecular network crystal structure thermal decomposition dehydration 


Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.


  1. Ben Ghozlen, M. H., Daoud, A., Paulus, H., & Pabst, I. (1994). Crystal structure of ethylenediammonium copper sulphate, [H3N(CH2)2NH3]Cu(SO4)2(H2O)4. Zeitschrift für Kristallographie — Crystalline Materials, 209, 383–383. DOI: 10.1524/zkri.1994.209.4.383.CrossRefGoogle Scholar
  2. Brandenburg, K., & Berndt, M. (2001). DIAMOND, Version 2.0. Bonn, Germany: Crystal Impact GbR.Google Scholar
  3. Chaabouni, S., Kamoun, S., Daoud, A., & Jouini, T. (1996). Manganese ethylenediammonium bis(sulfate) tetrahydrate. Acta Crystallographica Section C, 52, 505–506. DOI: 10.1107/s0108270195011048.CrossRefGoogle Scholar
  4. Coppens, P. (1970). The evaluation of absorption and extinction in single-crystal structure analysis. In F. R. Ahmed, S. R. Hall, & C. P. Huber (Eds.), Crystallographic Computing: Proceedings of an International Summer School organized by The Commission on Crystallographic Computing of the International Union of Crystallography, August 4–11, 1969, Ottava, Canada (pp. 255–270). Copenhagen, Denmark: Munksgaard Publishers.Google Scholar
  5. Farrugia, L. J. (1999). WinGX suite for small-molecule singlecrystal crystallography. Journal of Applied Crystallography, 32, 837–838. DOI: 10.1107/s0021889899006020.CrossRefGoogle Scholar
  6. Hajlaoui, F., Yahyaoui, S., Naïli, H., Mhiri, T., & Bataille, T. (2009). Synthesis, structural characterisation and thermal decomposition of a new organic-inorganic hybrid material (C5H14N2)[Cu(SO4)2(H2O)4] · H2O. Polyhedron, 28, 2113–2118. DOI: 10.1016/j.poly.2009.03.024.CrossRefGoogle Scholar
  7. Hajlaoui, F., Naïli, H., Yahyaoui, S., Turnbull, M. M., Mhiri, T., & Bataille, T. (2011). Synthesis, characterization and magnetic properties of four new organically templated metal sulfates [C5H14N2][MII(H2O)6](SO4)2, (MII = Mn, Fe, Co, Ni). Dalton Transactions, 40, 11613–11620. DOI: 10.1039/c1dt11030f.CrossRefGoogle Scholar
  8. Hajlaoui, F., Naïli, H., Yahyaoui, S., Norquist, A. J., Mhiri, T., & Bataille, T. (2012). Synthesis, crystal structures and thermal behaviour of organic-inorganic hybrids incorporating a chiral diamine. Journal of Organometallic Chemistry, 700, 110–116. DOI: 10.1016/j.jorganchem.2011.11.023.CrossRefGoogle Scholar
  9. Healy, P. C., Patrick, J. M., & White, A. H. (1984). Crystal structure of ethylenediammonium hexaaquanickel(II) sulfate: a variation on the Tutton salts. Australian Journal of Chemistry, 37, 1105–1109. DOI: 10.1071/ch9841105.CrossRefGoogle Scholar
  10. Held, P. (2003). Ethylenediammonium tetraaquabis(sulfato) iron(II). Acta Crystallographica Section E, 59, m197–m198. DOI: 10.1107/s1600536803004628.CrossRefGoogle Scholar
  11. Hill, C. L. (1998). Introduction: Polyoxometalatesmulticomponent molecular vehicles to probe fundamental issues and practical problems. Chemical Reviews, 98, 1–2. DOI: 10.1021/cr960395y.CrossRefGoogle Scholar
  12. Kagan, C. R., Mitzi, D. B., & Dimitrakopoulos, C. D. (1999). Organic-inorganic hybrid materials as semiconducting channels in thin-film field-effect transistors. Science, 286, 945–947. DOI: 10.1126/science.286.5441.945.CrossRefGoogle Scholar
  13. Naïli, H., Rekik, W., Bataille, T., & Mhiri, T. (2006). Crystal structure, phase transition and thermal behaviour of dabcodiium hexaaquacopper(II) bis(sulfate), (C6H14N2) [Cu(H2O)6](SO4)2. Polyhedron, 25, 3543–3554. DOI: 10.1016/j.poly.2006.07.010.CrossRefGoogle Scholar
  14. Nonius BV (1998). Kappa CCD program software. Delft, The Netherlands: Nonius BV.Google Scholar
  15. Otwinowski, Z., & Minor, W. (1997). Processing of X-ray diffraction data collected in oscillation mode. In C. W. Carter, Jr., & R. M. Sweet (Eds.), Macromolecular crystallography. Part A (Methods in Enzymology, Vol. 276, pp. 307–326). New York, NY, USA: Academic Press.Google Scholar
  16. Rekik, W., Naïli, H., Bataille, T., Roisnel, T., & Mhiri, T. (2006a). Supramolecular networks of transition metal sulfates templated by piperazine. Inorganica Chimica Acta, 359, 3954–3962. DOI: 10.1016/j.ica.2006.05.030.CrossRefGoogle Scholar
  17. Rekik, W., Naïli, H., Bataille, T., & Mhiri, T. (2006b). Synthesis, crystal structure, phase transition and thermal behaviour of a new dabcodiium hexaaquanickel(II) bis(sulphate), (C6H14N2)[Ni(H2O)6](SO4)2. Journal of Organometallic Chemistry, 691, 4725–4732. DOI: 10.1016/j.jorganchem.2006.07.019.CrossRefGoogle Scholar
  18. Rekik, W., Naïli, H., Mhiri, T., & Bataille, T. (2008). [NH3(CH2)2NH3][Co(SO4)2(H2O)4]: Chemical preparation, crystal structure, thermal decomposition and magnetic properties. Materials Research Bulletin, 43, 2709–2718. DOI: 10.1016/j.materresbull.2007.10.024.CrossRefGoogle Scholar
  19. Rekik, W., Naïli, H., Mhiri, T., & Bataille, T. (2012). Three organically templated magnesium sulfates: Chemical preparation, hydrogen-bonded structures and thermal behavior. Solid State Sciences, 14, 1503–1511. DOI: 10.1016/j.solidstatesciences.2012.08.027.CrossRefGoogle Scholar
  20. Rujiwatra, A., & Limtrakul, J. (2005). Ethane-1,2-diaminium hexaaquazinc(II) sulfate. Acta Crystallographica Section E, 61, m1403–m1404. DOI: 10.1107/s1600536805019604.CrossRefGoogle Scholar
  21. Rull, F., Pastor, J. M., & De Saja, J. A. (1977). Des anomalies observées dans l’étude par effet Raman de La2(SO4)3 · 9H2O monocristallin en fonction de la temperature. Solid State Communications, 21, 221–224. DOI: 10.1016/0038-1098(77)90689-5. (in French)CrossRefGoogle Scholar
  22. Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. Program for crystal structure resolution and analysis. Göttingen, Germany: University of Göttingen.Google Scholar
  23. Yahyaoui, S., Rekik, W., Naïli, H., Mhiri, T., & Bataille, T. (2007). Synthesis, crystal structures, phase transition characterization and thermal decomposition of a new dabcodiium hexaaquairon(II) bis(sulfate): (C6H14N2)[Fe(H2O)6](SO4)2. Journal of Solid State Chemistry, 180, 3560–3570. DOI: 10.1016/j.jssc.2007.10.019.CrossRefGoogle Scholar
  24. Wang, A., Freeman, J. J., Jolliff, B. L., & Chou, I. M. (2006). Sulfates on Mars: A systematic Raman spectroscopic study of hydration states of magnesium sulfates. Geochimica et Cosmochimica Acta, 70, 6118–6135. DOI:10.1016/j.gca.2006.05.022.CrossRefGoogle Scholar

Copyright information

© Institute of Chemistry, Slovak Academy of Sciences 2013

Authors and Affiliations

  • Dhouha ben Hassan
    • 1
  • Walid Rekik
    • 1
    Email author
  • Houcine Naïli
    • 1
  • Tahar Mhiri
    • 1
  1. 1.Laboratoire Physico-chimique de l’état Solide, Département de Chimie, Faculté des Sciences de SfaxUniversité de SfaxSfaxTunisie

Personalised recommendations