Synthesis, structure of [H3dien]·(MF6)·H2O (M=Cr, Fe) and Fe Mössbauer study of [H3dien]·(FeF6)·H2O |
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| Authors: | Amor Ben Ali,Minh Trang Dang,Annie Hé mon-Ribaud,Vincent Maisonneuve |
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| Affiliation: | a Laboratoire des Oxydes et Fluorures, UMR 6010 CNRS, Institut de Recherche en Ingénierie Moléculaire et Matériaux Fonctionnels, FR CNRS 2575, Faculté des Sciences et Techniques, Université du Maine, Avenue Olivier Messiaen, 72085 Le MANS Cedex 9, France
b Laboratoire de Physique de l’Etat Condensé, UMR 6087 CNRS, Institut de Recherche en Ingénierie Moléculaire et Matériaux Fonctionnels, FR CNRS 2575, Faculté des Sciences et Techniques, Université du Maine, Avenue Olivier Messiaen, 72085 Le MANS Cedex 9, France |
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| Abstract: | Single crystals of [H3dien]·(FeF6)·H2O (I) and [H3dien]·(CrF6)·H2O (II) are obtained by solvothermal synthesis under microwave heating. I is orthorhombic (Pna21) with a=11.530(2) Å, b=6.6446(8) Å, c=13.787(3) Å, V=1056.3(2) Å3 and Z=4. II is monoclinic (P21/c) with a=13.706(1) Å, b=6.7606(6) Å, c=11.3181(9) Å, β=99.38(1)°, V=1034.7(1) Å3 and Z=4. The structure determinations, performed from single crystal X-ray diffraction data, lead to the R1/wR2 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 FeF6 or CrF6 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 57Fe Mössbauer spectrometry: the hyperfine structure confirms the presence of Fe3+ in octahedral coordination and reveals the existence of paramagnetic spin fluctuations. |
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| Keywords: | Fluoride Fluoroferrate Fluorochromate Microwave heating Solvothermal synthesis Crystal structure Mö ssbauer spectrometry |
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