Synthesis and characterization of a new organic dihydrogenomonophosphate [3,5-(CH{sub 3}O){sub 2}C{sub 6}H{sub 3}NH{sub 3}]{sub 2}(H{sub 2}PO{sub 4}){sub 2}

doi:https://doi.org/10.1016/j.materresbull.2003.10.003

Title: Synthesis and characterization of a new organic dihydrogenomonophosphate [3,5-(CH{sub 3}O){sub 2}C{sub 6}H{sub 3}NH{sub 3}]{sub 2}(H{sub 2}PO{sub 4}){sub 2}

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Abstract

Chemical preparation, crystal structure, calorimetric studies and spectroscopic investigation are given for a new organic cation dihydrogenomonophosphate [3,5-(CH{sub 3}O){sub 2}C{sub 6}H{sub 3}NH{sub 3}]{sub 2}(H{sub 2}PO{sub 4}){sub 2}. This compound is triclinic P1-bar with the following unit cell parameters: a=9.030(6) A, b=16.124(5) A, c=8.868(3) A, {alpha}=75.04(3) deg., {beta}=110.71(4) deg., {gamma}=104.61(1) deg., Z=4, V=1148.0(1) A{sup 3}, Z=2 and {rho}{sub cal.}=1.454 g cm{sup -3}. Crystal structure was solved and refined to R=0.04, 2752 independent reflections. The atomic arrangement can be described as inorganic layers of H{sub 2}PO{sub 4}{sup -} anions parallel to y=((1)/(2)) planes, between which are located the organic groups. Solid-state {sup 13}C and {sup 31}P MAS-NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the attribution of the phosphorous and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups.

Authors:: Kaabi, K; Nasr, C Ben; Lefebvre, F

Publication Date:: 2004-02-02

OSTI Identifier:: 20888016

Resource Type:: Journal Article

Journal Name:: Materials Research Bulletin

Additional Journal Information:: Journal Volume: 39; Journal Issue: 2; Other Information: DOI: 10.1016/j.materresbull.2003.10.003; PII: S0025540803002976; Copyright (c) 2003 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0025-5408

Country of Publication:: United States

Language:: English

Subject:: 36 MATERIALS SCIENCE; ANIONS; CALORIMETRY; CARBON 13; CATIONS; CHEMICAL PREPARATION; CRYSTAL STRUCTURE; CRYSTALLOGRAPHY; LAYERS; NUCLEAR MAGNETIC RESONANCE; PHOSPHONATES; PHOSPHORUS 31; SPECTROSCOPY; X RADIATION; X-RAY DIFFRACTION

Citation Formats


                    Kaabi, K, Nasr, C Ben, and Lefebvre, F. Synthesis and characterization of a new organic dihydrogenomonophosphate [3,5-(CH{sub 3}O){sub 2}C{sub 6}H{sub 3}NH{sub 3}]{sub 2}(H{sub 2}PO{sub 4}){sub 2}.  United States: N. p., 2004. 
        Web.  doi:10.1016/j.materresbull.2003.10.003.

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                    Kaabi, K, Nasr, C Ben, & Lefebvre, F. Synthesis and characterization of a new organic dihydrogenomonophosphate [3,5-(CH{sub 3}O){sub 2}C{sub 6}H{sub 3}NH{sub 3}]{sub 2}(H{sub 2}PO{sub 4}){sub 2}.  United States.  https://doi.org/10.1016/j.materresbull.2003.10.003

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                    Kaabi, K, Nasr, C Ben, and Lefebvre, F. Mon .  
        "Synthesis and characterization of a new organic dihydrogenomonophosphate [3,5-(CH{sub 3}O){sub 2}C{sub 6}H{sub 3}NH{sub 3}]{sub 2}(H{sub 2}PO{sub 4}){sub 2}".  United States.  https://doi.org/10.1016/j.materresbull.2003.10.003.

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@article{osti_20888016,

  title        = {Synthesis and characterization of a new organic dihydrogenomonophosphate [3,5-(CH{sub 3}O){sub 2}C{sub 6}H{sub 3}NH{sub 3}]{sub 2}(H{sub 2}PO{sub 4}){sub 2}},

  author       = {Kaabi, K and Nasr, C Ben and Lefebvre, F},

  abstractNote = {Chemical preparation, crystal structure, calorimetric studies and spectroscopic investigation are given for a new organic cation dihydrogenomonophosphate [3,5-(CH{sub 3}O){sub 2}C{sub 6}H{sub 3}NH{sub 3}]{sub 2}(H{sub 2}PO{sub 4}){sub 2}. This compound is triclinic P1-bar with the following unit cell parameters: a=9.030(6) A, b=16.124(5) A, c=8.868(3) A, {alpha}=75.04(3) deg., {beta}=110.71(4) deg., {gamma}=104.61(1) deg., Z=4, V=1148.0(1) A{sup 3}, Z=2 and {rho}{sub cal.}=1.454 g cm{sup -3}. Crystal structure was solved and refined to R=0.04, 2752 independent reflections. The atomic arrangement can be described as inorganic layers of H{sub 2}PO{sub 4}{sup -} anions parallel to y=((1)/(2)) planes, between which are located the organic groups. Solid-state {sup 13}C and {sup 31}P MAS-NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the attribution of the phosphorous and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups.},

  doi          = {10.1016/j.materresbull.2003.10.003},

  url          = {https://www.osti.gov/biblio/20888016},
  journal      = {Materials Research Bulletin},

  issn         = {0025-5408},

  number       = 2,

  volume       = 39,

  place        = {United States},

  year         = {2004},

  month        = {2}

}

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