Sol-gel synthesis of K{sub 3}InF{sub 6} and structural characterization of K{sub 2}InC{sub 10}O{sub 10}H{sub 6}F{sub 9}, K{sub 3}InC{sub 12}O{sub 14}H{sub 4}F{sub 18} and K{sub 3}InC{sub 12}O{sub 12}F{sub 18}

Journal Article · Sat Oct 15 00:00:00 EDT 2005 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2005.08.002· OSTI ID:20721743

Labeguerie, Jessica ^[1]; Gredin, Patrick ^[1]; Marrot, Jerome ^[2]; Kozak, Ariel de ^[1]

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1. Laboratoire de Cristallochimie du Solide, Case courrier 176, UMR CNRS 7574, Universite Pierre-et-Marie-Curie, 4 place Jussieu, 75252 Paris, Cedex 05 (France)
2. Institut Lavoisier, UMR CNRS 8637, Universite de Versailles St-Quentin, 45 av. des Etats-Unis, 78035 Versailles, Cedex (France)

K{sub 3}InF{sub 6} is synthesized by a sol-gel route starting from indium and potassium acetates dissolved in isopropanol in the stoichiometry 1:3, with trifluoroacetic acid as fluorinating agent. The crystal structures of the organic precursors were solved by X-ray diffraction methods on single crystals. Three organic compounds were isolated and identified: K{sub 2}InC{sub 10}O{sub 10}H{sub 6}F{sub 9}, K{sub 3}InC{sub 12}O{sub 14}H{sub 4}F{sub 18} and K{sub 3}InC{sub 12}O{sub 12}F{sub 18}. The first one, deficient in potassium in comparison with the initial stoichiometry, is unstable. In its crystal structure, acetate as well as trifluoroacetate anions are coordinated to the indium atom. The two other precursors are obtained, respectively, by quick and slow evaporation of the solution. They correspond to the final organic compounds, which give K{sub 3}InF{sub 6} by decomposition at high temperature. The crystal structure of K{sub 3}InC{sub 12}O{sub 14}H{sub 4}F{sub 18} is characterized by complex anions [In(CF{sub 3}COO){sub 4}(OH{sub x}){sub 2}]{sup (5-2x)-} and isolated [CF{sub 3}COOH{sub 2-x}]{sup (x-1)-} molecules with x=2 or 1, surrounded by K{sup +} cations. The crystal structure of K{sub 3}InC{sub 12}O{sub 12}F{sub 18} is only constituted by complex anions [In(CF{sub 3}COO){sub 6}]{sup 3-} and K{sup +} cations. For all these compounds, potassium cations ensure only the electroneutrality of the structure. IR spectra of K{sub 2}InC{sub 10}O{sub 10}H{sub 6}F{sub 9} and K{sub 3}InC{sub 12}O{sub 12}F{sub 18} were also performed at room temperature on pulverized crystals.

• OSTI ID: 20721743
• Journal Information: Journal of Solid State Chemistry, Vol. 178, Issue 10; Other Information: DOI: 10.1016/j.jssc.2005.08.002; PII: S0022-4596(05)00352-X; Copyright (c) 2005 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ACETATES
ANIONS
CATIONS
CRYSTAL STRUCTURE
DECOMPOSITION
EVAPORATION
INDIUM FLUORIDES
INFRARED SPECTRA
MONOCRYSTALS
ORGANOMETALLIC COMPOUNDS
POTASSIUM FLUORIDES
POTASSIUM IONS
SOL-GEL PROCESS
STOICHIOMETRY
SYNTHESIS
TEMPERATURE RANGE 0273-0400 K
X-RAY DIFFRACTION