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Inorganic–organic hybrid materials: synthesis and crystal structure determination from powder diffraction data of Pb2(O3PCH2C6H4CH2PO3)

Authors
Journal
Journal of Solid State Chemistry
0022-4596
Publisher
Elsevier
Publication Date
Volume
173
Issue
2
Identifiers
DOI: 10.1016/s0022-4596(03)00085-9
Keywords
  • Lead
  • Phosphonate
  • Hybrid Material
  • Hydrothermal Synthesis
  • Ir Spectroscopy
  • X-Ray Diffraction
  • Rietveld Refinement
Disciplines
  • Earth Science
  • Geography

Abstract

Abstract A new lead diphosphonate, Pb 2(O 3PCH 2C 6H 4CH 2PO 3) was hydrothermally synthesized from tetraethyl α, α′- p-xylenediphos-phonate and Pb(NO 3) 2. The structure was solved and refined using X-ray powder diffraction data. It crystallizes in the monoclinic space group P2 1/ c, with a = 467.84(2), b = 2007.98(9), c = 639.10(2) pm, β = 101.020(3)°, V = 589.31(4) 10 6 pm, Z=2, w R p=0.034, R p=0.027, R F2=0.061, R F=0.036. The structure is built from corner-linked [PbO 4] polyhedra, containing a lone pair of electrons. These polyhedra are connected to layers by phosphonate groups, RPO 3 2− and through the organic diphosphonic acid to a three-dimensional structure. Thermogravimetric as well as IR spectroscopic studies are also presented.

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