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

Journal Article · Wed Dec 15 00:00:00 EST 2010 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2010.09.008· OSTI ID:21494133

Mi, Jin-Xiao ^[1]; Wang, Cheng-Xin ^[1]; Chen, Ning ^[2]; Li, Rong ^[1]; Pan, Yuanming ^[3]

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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. Department of Geological Sciences, University of Saskatchewan, Saskatoon, SK, Canada S7N 5E2 (Canada)

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) octahedra linked by PO{sub 4} tetrahedra. Display Omitted

• OSTI ID: 21494133
• Journal Information: Journal of Solid State Chemistry, Vol. 183, 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.; ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

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