The crystal structure of manganese sulfate templated by 1,4-diaza-bicyclo[2.2.2]octane (abbreviated dabco), (C6H14N2)[Mn(H2O)6](SO4)2, was investigated using single crystal X-ray diffraction data. It crystallises in the monoclinic system (space group P21/c) with the following unit-cell parameters: a = 12.1392(2) Å, b = 12.3117(2) Å, c = 12.2765(2) Å, β = 104.607(1)°, V = 1775.47(5) Å3 and Z = 4. The structure has been solved using direct methods and refined by least-squares analysis [R 1 = 0.0381, wR 2 = 0.1082]. The crystal structure of the title compound is built from isolated [Mn(H2O)6]2+ octahedral cations, 1,4-diaza-bicyclo[2.2.2]octandiium cations (C6H14N2)2+ and sulfate anions (SO4)2− connected by a three-dimensional hydrogen-bond network. The thermal decomposition of the precursor, studied by thermogravimetry and temperature-dependent X-ray powder diffraction, proceeds through four stages giving rise to the mixture of Mn2O3and Mn3O4.
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Cheetham, A.K.; Férey, G.; Loiseau, T. Angew. Chem., Int. Ed. 1999, 38, 3269.
Gier, T.E.; Stucky, G.D. Nature 1991, 349, 508; Férey, G. J. Fluorine Chem. 1995, 72, 187; Khan, M.I.; Meyer, L.M.; Haushalter, R.C.; Schweitzer, A.L.; Zubieta, J.; Dye, J.L. Chem. Mater. 1996, 8, 43.
Breck, D.W. Zeolite Molecular Sieves: Structure, Chemistry and Use; Wiley and Sons: London, 1974; Clearfield A. Chem. Rev. 1988, 88, 125; Venuto, P.B. Microporous Mater. 1994, 2, 297.
Khan, M.I.; Cevik, S.; Doedens, R.J. Inorg. Chim. Acta 1999, 292, 112.
Choudhury, A., Krishnamoorthy, J.; Rao, C.N.R. Chem. Commun. 2001, 2610.
Bull, I.; Wheatley, P.S.; Lightfoot, P.; Morris, R.E.; Sastre, E.; Wright, P.A. Chem. Commun. 2002, 1180.
Rao, C.N.R.; Behera, J.N.; Dan, M. Chem. Soc. Rev. 2006, 35, 375.
Bataille, T.; Louër, D. J. Mater. Chem. 2002, 12, 3487.
Bataille, T.; Louër, D. J. Solid State Chem. 2004, 177, 1235.
Thomas, P.M.; Norquist, A.J.; Doran, M.B.; O’Hare, D. J. Mater. Chem. 2003, 13, 88.
Norquist, A.J.; Thomas, P.M.; Doran, M.B.; O’Hare, D. Chem. Mater. 2002, 14, 5179.
Doran, M.B.; Norquist, A.J.; O’Hare, D. Chem. Commun. 2002, 2946.
Norquist, A.J.; Doran, M.B.; Thomas, P.M.; O’Hare, D. Dalton Trans. 2003, 1168.
Bataille, T. Acta Crystallogr. 2003, C59, m459.
Pan, J.-X.; Yang, G.-Y.; Sun, Y.-Q. Acta Crystallogr. 2003, E59, m286.
Fleck, M.; Bohaty, L.; Tillmanns, E. Solid State Sci. 2004, 6, 469.
Rekik, W.; Naïli, H.; Mhiri, T.; Bataille, T. Acta Crystallogr. 2005, E61, m629.
Rekik, W.; Naïli, H.; Bataille, T.; Roisnel, T.; Mhiri, T. Inorg. Chim. Acta 2006, 359, 3954.
Rekik, W.; Naïli, H.; Bataille, T.; Mhiri, T. J. Organomet. Chem. 2006, 691, 4725.
Naïli, H.; Rekik, W.; Bataille, T.; Mhiri, T. Polyhedron 2006, in press.
Zhao, Y.-J.; Li, X.-H.; Wang, S. Acta Crystallogr. 2005, E61, m671.
Held, P. Acta Crystallogr. 2003, E59, m197.
Nonius. Kappa CCD Program Software, Nonius BV, Delft, The Netherlands, 1998.
Otwinowski, Z.; Minor, W.; Carter, C.W.; Sweet, R.M. (Eds.). Methods in Enzymology; Academic Press: New York, 1997; vol. 276, p. 307.
De Meulenaer, J.; Tompa, H. Acta Crystallogr. 1965, 19, 1014.
Farrugia, L.J. J. Appl. Crystallogr. 1999, 32, 837.
Sheldrick, G.M. SHELXS-97, Program for Crystal Structure Solution; University of Göttingen: Germany, 1997.
Sheldrick, G.M. SHELXL-97, Program for Crystal Structure Refinement; University of Göttingen: Germany, 1997.
Paul, G.; Choudhury, A.; Rao, C.N.R. Chem. Mater. 2003, 15, 1174.
Brown, I.D. J. Appl. Crystallogr. 1996, 29, 479.
Jayaraman, K.; Choudhury, A.; Rao, C.N.R. Solid State Sci. 2002, 4, 413.
Paul, G.; Choudhury, A.; Nagarajan, R.; Rao, C.N.R. Inorg. Chem. 2003, 42, 2004.
Zaki, M.I.; Hasan, M.A.; Pasupulety, L.; Kumari, K. Thermochim. Acta 1997, 303, 171.
Acknowledgment
Grateful thanks are expressed to Dr. T. Roisnel (Centre de Diffractométrie X, UMR CNRS 6226) and Mr. G. Marsolier for their assistance in single-crystal and powder X-ray diffraction data collection, respectively.
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Supplementary Material CCDC 620298 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
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Rekik, W., Naïli, H., Mhiri, T. et al. A new dabco templated metal sulfate, (C6H14N2)[Mn (H2O)6](SO4)2. Chemical preparation, hydrogen-bonded structure and thermal decomposition. J Chem Crystallogr 37, 147–155 (2007). https://doi.org/10.1007/s10870-006-9170-9
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DOI: https://doi.org/10.1007/s10870-006-9170-9