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Title: Synthesis, structure of [H{sub 3} dien].(MF{sub 6}).H{sub 2}O (M=Cr, Fe) and {sup 57}Fe Moessbauer study of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O

Abstract

Single crystals of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O (I) and [H{sub 3} dien].(CrF{sub 6}).H{sub 2}O (II) are obtained by solvothermal synthesis under microwave heating. I is orthorhombic (Pna2{sub 1}) with a=11.530(2) A, b=6.6446(8) A, c=13.787(3) A, V=1056.3(2) A{sup 3} and Z=4. II is monoclinic (P2{sub 1} /c) with a=13.706(1) A, b=6.7606(6) A, c=11.3181(9) A, {beta}=99.38(1){sup o}, V=1034.7(1) A{sup 3} and Z=4. The structure determinations, performed from single crystal X-ray diffraction data, lead to the R {sub 1}/wR {sub 2} reliability factors 0.028/0.066 for I and 0.035/0.102 for II. The structures of I and II are built up from isolated FeF{sub 6} or CrF{sub 6} octahedra, water molecules and triprotonated amines. In both structures, each octahedron is connected by hydrogen bonds to six organic cations and two water molecules. The iron-based compound is also characterized by {sup 57}Fe Moessbauer spectrometry: the hyperfine structure confirms the presence of Fe{sup 3+} in octahedral coordination and reveals the existence of paramagnetic spin fluctuations. - Graphical abstract: Moessbauer spectra of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O.

Authors:
 [1];  [2];  [1];  [1];  [1]
  1. Laboratoire des Oxydes et Fluorures, UMR 6010 CNRS, Institut de Recherche en Ingenierie Moleculaire et Materiaux Fonctionnels, FR CNRS 2575, Faculte des Sciences et Techniques, Universite du Maine, Avenue Olivier Messiaen, 72085 Le MANS Cedex 9 (France)
  2. Laboratoire de Physique de l'Etat Condense, UMR 6087 CNRS, Institut de Recherche en Ingenierie Moleculaire et Materiaux Fonctionnels, FR CNRS 2575, Faculte des Sciences et Techniques, Universite du Maine, Avenue Olivier Messiaen, 72085 Le MANS Cedex 9 (France)
Publication Date:
OSTI Identifier:
21015854
Resource Type:
Journal Article
Journal Name:
Journal of Solid State Chemistry
Additional Journal Information:
Journal Volume: 180; Journal Issue: 6; Other Information: DOI: 10.1016/j.jssc.2007.03.030; PII: S0022-4596(07)00135-1; Copyright (c) 2007 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0022-4596
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; AMINES; CHROMIUM FLUORIDES; HYPERFINE STRUCTURE; IRON FLUORIDES; IRON IONS; MICROWAVE HEATING; MOESSBAUER EFFECT; MONOCLINIC LATTICES; MONOCRYSTALS; ORTHORHOMBIC LATTICES; PARAMAGNETISM; SPIN; SYNTHESIS; X-RAY DIFFRACTION

Citation Formats

Ben Ali, Amor, Trang Dang, Minh, Greneche, Jean-Marc, Hemon-Ribaud, Annie, Leblanc, Marc, and Maisonneuve, Vincent. Synthesis, structure of [H{sub 3} dien].(MF{sub 6}).H{sub 2}O (M=Cr, Fe) and {sup 57}Fe Moessbauer study of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O. United States: N. p., 2007. Web. doi:10.1016/j.jssc.2007.03.030.
Ben Ali, Amor, Trang Dang, Minh, Greneche, Jean-Marc, Hemon-Ribaud, Annie, Leblanc, Marc, & Maisonneuve, Vincent. Synthesis, structure of [H{sub 3} dien].(MF{sub 6}).H{sub 2}O (M=Cr, Fe) and {sup 57}Fe Moessbauer study of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O. United States. https://doi.org/10.1016/j.jssc.2007.03.030
Ben Ali, Amor, Trang Dang, Minh, Greneche, Jean-Marc, Hemon-Ribaud, Annie, Leblanc, Marc, and Maisonneuve, Vincent. 2007. "Synthesis, structure of [H{sub 3} dien].(MF{sub 6}).H{sub 2}O (M=Cr, Fe) and {sup 57}Fe Moessbauer study of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O". United States. https://doi.org/10.1016/j.jssc.2007.03.030.
@article{osti_21015854,
title = {Synthesis, structure of [H{sub 3} dien].(MF{sub 6}).H{sub 2}O (M=Cr, Fe) and {sup 57}Fe Moessbauer study of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O},
author = {Ben Ali, Amor and Trang Dang, Minh and Greneche, Jean-Marc and Hemon-Ribaud, Annie and Leblanc, Marc and Maisonneuve, Vincent},
abstractNote = {Single crystals of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O (I) and [H{sub 3} dien].(CrF{sub 6}).H{sub 2}O (II) are obtained by solvothermal synthesis under microwave heating. I is orthorhombic (Pna2{sub 1}) with a=11.530(2) A, b=6.6446(8) A, c=13.787(3) A, V=1056.3(2) A{sup 3} and Z=4. II is monoclinic (P2{sub 1} /c) with a=13.706(1) A, b=6.7606(6) A, c=11.3181(9) A, {beta}=99.38(1){sup o}, V=1034.7(1) A{sup 3} and Z=4. The structure determinations, performed from single crystal X-ray diffraction data, lead to the R {sub 1}/wR {sub 2} reliability factors 0.028/0.066 for I and 0.035/0.102 for II. The structures of I and II are built up from isolated FeF{sub 6} or CrF{sub 6} octahedra, water molecules and triprotonated amines. In both structures, each octahedron is connected by hydrogen bonds to six organic cations and two water molecules. The iron-based compound is also characterized by {sup 57}Fe Moessbauer spectrometry: the hyperfine structure confirms the presence of Fe{sup 3+} in octahedral coordination and reveals the existence of paramagnetic spin fluctuations. - Graphical abstract: Moessbauer spectra of [H{sub 3} dien].(FeF{sub 6}).H{sub 2}O.},
doi = {10.1016/j.jssc.2007.03.030},
url = {https://www.osti.gov/biblio/21015854}, journal = {Journal of Solid State Chemistry},
issn = {0022-4596},
number = 6,
volume = 180,
place = {United States},
year = {Fri Jun 15 00:00:00 EDT 2007},
month = {Fri Jun 15 00:00:00 EDT 2007}
}