A new organically templated magnesium sulfate: structure, spectroscopic analysis, and thermal behaviour
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Dhouha Hassan
,
Walid Rekik
Abstract
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.
[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. http://dx.doi.org/10.1524/zkri.1994.209.4.38310.1524/zkri.1994.209.4.383Suche in Google Scholar
[2] Brandenburg, K., & Berndt, M. (2001). DIAMOND, Version 2.0. Bonn, Germany: Crystal Impact GbR. Suche in 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. http://dx.doi.org/10.1107/S010876819501291210.1107/S0108270195011048Suche in Google 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. Suche in 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. http://dx.doi.org/10.1107/S002188989900602010.1107/S0021889899006020Suche in Google 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. http://dx.doi.org/10.1016/j.poly.2009.03.02410.1016/j.poly.2009.03.024Suche in Google 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. http://dx.doi.org/10.1039/c1dt11030f10.1039/c1dt11030fSuche in Google Scholar PubMed
[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. http://dx.doi.org/10.1016/j.jorganchem.2011.11.02310.1016/j.jorganchem.2011.11.023Suche in Google 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. http://dx.doi.org/10.1071/CH984110510.1071/CH9841105Suche in Google Scholar
[10] Held, P. (2003). Ethylenediammonium tetraaquabis(sulfato) iron(II). Acta Crystallographica Section E, 59, m197–m198. DOI: 10.1107/s1600536803004628. http://dx.doi.org/10.1107/S160053680300462810.1107/S1600536803004628Suche in Google 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. http://dx.doi.org/10.1021/cr960395y10.1021/cr960395ySuche in Google Scholar PubMed
[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. http://dx.doi.org/10.1126/science.286.5441.94510.1126/science.286.5441.945Suche in Google Scholar PubMed
[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. http://dx.doi.org/10.1016/j.poly.2006.07.01010.1016/j.poly.2006.07.010Suche in Google Scholar
[14] Nonius BV (1998). Kappa CCD program software. Delft, The Netherlands: Nonius BV. Suche in 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. Suche in 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. http://dx.doi.org/10.1016/j.ica.2006.05.03010.1016/j.ica.2006.05.030Suche in Google 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. http://dx.doi.org/10.1016/j.jorganchem.2006.07.01910.1016/j.jorganchem.2006.07.019Suche in Google 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. http://dx.doi.org/10.1016/j.materresbull.2007.10.02410.1016/j.materresbull.2007.10.024Suche in Google 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. http://dx.doi.org/10.1016/j.solidstatesciences.2012.08.02710.1016/j.solidstatesciences.2012.08.027Suche in Google 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. http://dx.doi.org/10.1107/S160053680501960410.1107/S1600536805019604Suche in Google 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) http://dx.doi.org/10.1016/0038-1098(77)90689-510.1016/0038-1098(77)90689-5Suche in Google Scholar
[22] Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. Program for crystal structure resolution and analysis. Göttingen, Germany: University of Göttingen. Suche in 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. http://dx.doi.org/10.1016/j.jssc.2007.10.01910.1016/j.jssc.2007.10.019Suche in Google 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. http://dx.doi.org/10.1016/j.gca.2006.05.02210.1016/j.gca.2006.05.022Suche in Google Scholar
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