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Title: Synthesis and crystal structure of a new open-framework iron phosphate (NH{sub 4}){sub 4}Fe{sub 3}(OH){sub 2}F{sub 2}[H{sub 3}(PO{sub 4}){sub 4}]: Novel linear trimer of corner-sharing Fe(III) octahedra

A new iron phosphate (NH{sub 4}){sub 4}Fe{sub 3}(OH){sub 2}F{sub 2}[H{sub 3}(PO{sub 4}){sub 4}] has been synthesized hydrothermally at HF concentrations from 0.5 to 1.2 mL. Single-crystal X-ray diffraction analysis reveals its three-dimensional open-framework structure (monoclinic, space group P2{sub 1}/n (No. 14), a=6.2614(13) A, b=9.844(2) A, c=14.271(3) A, {beta}=92.11(1){sup o}, V=879.0(3) A{sup 3}). This structure is built from isolated linear trimers of corner-sharing Fe(III) octahedra, which are linked by (PO{sub 4}) groups to form ten-membered-ring channels along [1 0 0]. This isolated, linear trimer of corner-sharing Fe(III) octahedra, [(FeO{sub 4}){sub 3}(OH){sub 2}F{sub 2}], is new and adds to the diverse linkages of Fe polyhedra as secondary building units in iron phosphates. The trivalent iron at octahedral sites for the title compound has been confirmed by synchrotron Fe K-edge XANES spectra and magnetic measurements. Magnetic measurements also show that this compound exhibit a strong antiferromagnetic exchange below T{sub N}=17 K, consistent with superexchange interactions expected for the linear trimer of ferric octahedra with the Fe-F-Fe angle of 132.5{sup o}. -- Graphical abstract: The three-dimensional open-framework structure of (NH{sub 4}){sub 4}Fe{sub 3}(OH){sub 2}F{sub 2}[H{sub 3}(PO{sub 4}){sub 4}] is built from a novel isolated, linear (FeO{sub 4}){sub 3}(OH){sub 2}F{sub 2} trimer of corner-sharing Fe(III)more » octahedra linked by PO{sub 4} tetrahedra. Display Omitted« less
Authors:
 [1] ;  [1] ;  [2] ;  [3] ;  [1] ;  [3] ;  [4]
  1. Department of Materials Science and Engineering, College of Materials, Xiamen University, Xiamen 361005 (China)
  2. Canadian Light Source, University of Saskatchewan, Saskatoon, SK, Canada S7N 0X4 (Canada)
  3. (Canada)
  4. Department of Geological Sciences, University of Saskatchewan, Saskatoon, SK, Canada S7N 5E2 (Canada)
Publication Date:
OSTI Identifier:
21494133
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 183; Journal Issue: 12; Other Information: DOI: 10.1016/j.jssc.2010.09.008; PII: S0022-4596(10)00394-4; Copyright (c) 2010 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ABSORPTION SPECTROSCOPY; ANTIFERROMAGNETISM; HYDROFLUORIC ACID; HYDROTHERMAL SYNTHESIS; IRON OXIDES; IRON PHOSPHATES; MAGNETIC PROPERTIES; MONOCLINIC LATTICES; MONOCRYSTALS; SPACE GROUPS; SPECTRA; X-RAY DIFFRACTION; X-RAY SPECTROSCOPY CHALCOGENIDES; COHERENT SCATTERING; CRYSTAL LATTICES; CRYSTAL STRUCTURE; CRYSTALS; DIFFRACTION; FLUORINE COMPOUNDS; HALOGEN COMPOUNDS; HYDROGEN COMPOUNDS; INORGANIC ACIDS; INORGANIC COMPOUNDS; IRON COMPOUNDS; MAGNETISM; OXIDES; OXYGEN COMPOUNDS; PHOSPHATES; PHOSPHORUS COMPOUNDS; PHYSICAL PROPERTIES; SCATTERING; SPECTROSCOPY; SYMMETRY GROUPS; SYNTHESIS; TRANSITION ELEMENT COMPOUNDS