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Ionothernnal Synthesis, Structures, and Magnetism of Three New Open Framework Iron Halide-Phosphates
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Łukasiewicz Research Network-PORT Polish Center for Technology Development, Poland.ORCID iD: 0000-0002-1730-0304
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Number of Authors: 62019 (English)In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 58, no 19, p. 13203-13212Article in journal (Refereed) Published
Abstract [en]

A set of different open framework iron phosphates have been synthesized ionothermally using a task-specific ionic liquid, 1-butyl-4-methylpyridinium hexafluorophosphate, that acts in the synthesis as the reaction medium and mineralizer: (NH4)(2)Fe-2(HPO4)(PO4)Cl2F (1) and K2Fe2(HPO4(PO4)Cl2F (2) exhibit similar composition and closely related structural features. Both structures consist of {Fe-2(HPO4)(PO4)-Cl2F}(2)- macroanions and charge balancing ammonium or potassium cations. Their open framework structure contains layers and chains of corner-linked {Fe(1)O2Cl4} and {Fe(2)F2O4} octahedra, respectively, interconnected by PO4 tetrahedra forming 10-ring channels. KFe(PO3F)F-2 (3) is built up by {Fe[(PO3F)(4/3)F-2/2]}{Fe(PO3F)(2/3) F2/2F2} layers separated by K+ cations. Chains of alternating {FeF2O4} and {FeO2F4} octahedra, which are linear for 1 but undulated for 2, are linked to each other via corner-sharing {PO3F} tetrahedra with the fluorine pointing into the interlayer space. The compounds were characterized by means of single crystal and powder X-ray diffraction, infrared spectroscopy, and magnetic measurements. 1 reveals a strong ground state spin anisotropy with a spin 5/2 state and a magnetic moment of 5.3 mu(B) /Fe3+. Specific heat and magnetic data unveil three magnetic transitions at 95, 50, and 3.6 K. Compound 2 has a very similar crystal structure as compared to 1 but exhibits a different magnetic behavior: a slightly lower magnetic moment of 4.7 mu(B)/Fe3+ and a magnetic transition to a canted antiferromagnetic state below 90 K. Compound 3 exhibits typical paramagnetic behavior close to room-temperature (5.71 mu(B)/Fe3+). There are no clear indications for a phase transition down to 2 K despite strong antiferromagnetic spin-spin interactions; only a magnetic anomaly appears at 50 K in the zero-field cooled data.

Place, publisher, year, edition, pages
2019. Vol. 58, no 19, p. 13203-13212
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Chemical Sciences
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URN: urn:nbn:se:su:diva-175815DOI: 10.1021/acs.inorgchem.9b02028ISI: 000489676400081PubMedID: 31539232OAI: oai:DiVA.org:su-175815DiVA, id: diva2:1371738
Available from: 2019-11-20 Created: 2019-11-20 Last updated: 2019-11-20Bibliographically approved

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Siebeneichler, StefanieWilk-Kozubek, MagdalenaSmetana, VolodymyrMudring, Anja-Verena
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