[H3tren] templated iron fluorides; synthesis, crystal structures and Mössbauer studies |
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| Authors: | Amor Ben Ali Jean-Marc Grenche Marc Leblanc Vincent Maisonneuve |
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| Institution: | Amor Ben Ali, Jean-Marc Grenèche, Marc Leblanc,Vincent Maisonneuve |
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| Abstract: | The hydrothermal synthesis, using tris-(2-ethylamino)amine (tren) as a template, and the crystal structures of three new hybrid iron fluorides, (H3O)2·H3tren]2·(FeF6)2·(FeF5(H2O))·2H2O (I), H3tren]2·(FeF6)2·(FeF2(H2O)4)·8H2O (II) and H3tren]2·(FeF6)·(F)3·H2O (III), are reported. I, II, and III are triclinic (P-1), monoclinic (P21/c) and orthorhombic (I222), respectively. The structure of I is built up from isolated FeF6 and FeF5(H2O) distorted octahedra separated by triprotonated H3tren]3+ cations, disordered H3O+ cations and H2O molecules. In II, FeIIIF6 and neutral FeIIF2(H2O)4] octahedra form, together with H3tren]3+ cations, infinite (100) layers separated by extra water molecules. The structure of III consists of isolated and disordered FeF6 octahedra, fluoride anions F− connected to H3tren]3+ cations and extra fluoride anions F− disordered with H2O molecules. All H3tren]3+ cations have a “spider” type conformation. 57Fe Mössbauer characterization shows that +III valence state can only be considered for iron cations in I and III and preliminary Mössbauer results are consistent with the presence of both +II and +III valences for iron cations in II, in agreement with the crystallographic results. |
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| Keywords: | Fluoride Iron Microwave heating Solvothermal synthesis Structure 57Fe Mö ssbauer spectrometry |
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