Synthesis, crystal structure and characterization of a new octane-1,8-diammonium bis(dihydrogenmonophosphate)


The synthesis and the structure of a new [H3N-(CH2)8-NH3][H2PO4]2 is described. This compound crystallizes in the orthorhombic system, with the centric space group Pbcn and the following unit cell parameters: a = 7.2887 (4), b = 9.1728 (6), c = 23.2169 (19) Å, Z = 4 and V = 1552.23 (18) Å3. The crystal structure has been solved and refined to R = 0.074 and R(w) = 0.173. The [H2PO4]- entities are associated by O---H...O strong hydrogen bonds to form layers. These latters are interconnected with the organic entities via (N)-H...O hydrogen bonds. In this atomic arrangement, H bonds between the different species play an important role in the three-dimensional network. This compound has also been characterized by infrared spectroscopy, solid state MAS-NMR and thermal analysis.

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Mrad, M. , Ammar, S. , Ferretti, V. , Rzaigui, M. and Nasr, C. (2011) Synthesis, crystal structure and characterization of a new octane-1,8-diammonium bis(dihydrogenmonophosphate). Open Journal of Inorganic Chemistry, 1, 1-8. doi: 10.4236/ojic.2011.11001.

Conflicts of Interest

The authors declare no conflicts of interest.


[1] Evans, O.R. and Lin, W.B. (2002) Crystal engineering of NLO materials based on metal-organic coordination networks. Accounts of Chemical Research, 35, 511-522. doi:10.1021/ar0001012
[2] Zhang, J.P. and Chen, X.M. (2006) Crystal engineering of binary metal imidazolate and triazolate frameworks. Chemical Communications, 2006, 1689-1699. doi:10.1039/b516367f
[3] Steiner, T. (2002) The hydrogen bond in the solid state. Angewandte Chemie International Edition, 41, 48-76. doi:10.1002/1521-3773(20020104)41:1<48::AID-ANIE48>3.0.CO;2-U
[4] Jayaraman, K., Choudhury, A. and Rao, C.N.R. (2002) Sulfates of organic diamines: Hydrogen-bonded structures and properties. Solid State Sciences, 4, 413-422. doi:10.1016/S1293-2558(02)01269-4
[5] Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori, G. and Spagna, R. (1999) SIR97: A new tool for crystal structure determination and refinement. Journal of Applied Crystallography, 32, 115-119. doi:10.1107/S0021889898007717
[6] Sheldrick, G.M. (1997) SHELXL-97, program for crystal structure refinement, University of G?ttingen, G?ttingen, Germany.
[7] Farrugia, L.J. (1999) WinGX suite for small-molecule single-crystal crystallography. Journal of Applied Crystallography, 32, 837-838. doi:10.1107/S0021889899006020
[8] Brandenburg, K. (1998) Diamond Version 2.0 Impact GbR, Bonn, Germany.
[9] Burnett, M.N. and Johnson C.K. (1996) ORTEPIII. Report ORNL-6895, Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA.
[10] Herzfeld, J. and Berger, A.E. (1980) Sideband intensities in NMR spectra of samples spinning at the magic angle. Journal of Chemical Physics, 73, 6021-6030.
[11] Mrad, M.L., Ben Nasr, C. and Rzaigui, M. (2006) Synthesis and characterization of a new p-phenylenediammonium dihydrogenmonophosphate [p-NH3C6H4NH3] [H2PO4]2. Materials Research Bulletin, 41, 1287-1294. doi:10.1016/j.materresbull.2006.01.002
[12] Oueslati, A. and Ben Nasr, C. (2006) Synthesis and cry- stal structure of a new organic 2-amino-5-chloro pyridi- nium dihydrogenmonophosphate: (2-NH2-5-Cl-C5H3NH) H2PO4. Analytical Sciences: X-ray Structure Analysis Online, 22, 225-226.
[13] Hartmann, P., Vogel, J. and Schnabel, B. (1994) The influence of short-range geometry on the 31P chemical-shift tensor in protonated phosphates. Journal of Magnetic Resonance, Series A, 111, 110-114. doi:10.1006/jmra.1994.1234
[14] Kaabi, K., Rayes, A., Ben Nasr, C., Rzaigui, M. and Lefebvre, F. (2003) Synthesis and crystal sructure of a new dihydrogenomonophosphate (4-C2H5C6H4NH3)- H2PO4. Materials Research Bulletin, 38, 741-747. doi:10.1016/S0025-5408(03)00072-2
[15] Oueslati, A., Touati, A., Ben Nasr, C. and Lefebvre, F. (2006) The synthesis and characterization of 2-amino-3-methylpyridinium dihydrogenmonophosphate: (C6H9N2)-H2PO4. Phosphorus, Sulfur, and Silicon and the Related Elements, 181, 2117-2133. doi:10.1080/10426500600614196
[16] Kefi, R., Rayes, A., Ben Nasr, C. and Rzaigui, M. (2006) Synthesis and characterization of a new monophosphate (5-Cl-2,4-(OCH3)2C6H2NH3)H2PO4. Materials Research Bulletin, 42, 404-412. doi:10.1016/j.materresbull.2006.07.007
[17] Oueslati, J., Oueslati, A., Ben Nasr, C. and Lefebvre, F. (2006) Synthesis and crystal structure of a new adduct of dihydrogenphosphate phosphoric acid monohydrate with 8-aminoquinolinium (8-NH2C9H6NH)2(H2PO4)2H3PO4.H2O. Solid State Sciences, 8, 1067-1073. doi:10.1016/j.solidstatesciences.2006.03.005
[18] Kefi, R., Ben Nasr, C. and Lefebvre, F. (2007) Synthesis and characterization of a layered chlorozincophosphate templated by protonated 4-methylpiperidine. Crystal Research and Technology, 42, 333-341. doi:10.1002/crat.200610824
[19] Naili, H., Mhiri, T. and Daoud, A. (2001) Structural, vibrational and calorimetric study of a new ammonium dihydrogen phosphate-arsenate: NH4H2(PO4)0.52(AsO4)0.48. International Journal of Inorganic Materials, 3, 393-400. doi:10.1016/S1466-6049(01)00022-8
[20] Nemec, I., Cisarova, I. and Micka, Z.J. (1998) Study of the family of glycine-selenious acid addition compounds: crystal structure of diglycine hydrogen selenite and vibrational spectra and DSC measurement of diglycine hydrogen selenite and monoglycine-selenious acid crystals. Journal of Solid State Chemistry, 140, 71-82. doi:10.1006/jssc.1998.7855
[21] Haile, S.M., Calkins, P.M. and Boysen, D. (1998) Structure and vibrational spectrum of β-Cs3(HSO4)2[H2-x(P1-x, Sx)O4] (x~0.5), a new superprotonic conductor, and a comparison with α-Cs3(HSO4)2(H2PO4). Journal of Solid State Chemistry, 139, 373-387. doi:10.1006/jssc.1998.7861

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