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Ethanol- and Methanol-Coordinated and Solvent-Free Dodecahydro closo-Dodecaborates of 3d Transition Metals and of Magnesium

1
Department of Quantum Matter Physics, Laboratory of Crystallography, University of Geneva, Quai Ernest Ansermet 24, CH-1211 Geneva, Switzerland
2
Polish Academy of Sciences, Institute of Nuclear Physics, ul. Radzikowskiego 152, 31-342 Kraków, Poland
*
Author to whom correspondence should be addressed.
Crystals 2019, 9(7), 372; https://doi.org/10.3390/cryst9070372
Received: 25 June 2019 / Revised: 16 July 2019 / Accepted: 19 July 2019 / Published: 21 July 2019
(This article belongs to the Section Crystalline Materials)
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Abstract

Magnesium and 3d transition metals closo-borates were prepared by mechanosynthesis (ball milling) of the mixtures Na2B12H12 + MCl2 (M = Mn, Fe, Co, Ni, Mg), followed by addition of ethanol or methanol and drying under dynamic vacuum. The dead mass of NaCl is partly removed by filtration. The crystal structures of solvent-coordinated and solvent-free closo-borates have been characterized by temperature dependent synchrotron radiation X-ray powder diffraction, ab initio calculations, thermal analysis and infrared spectroscopy. Various solvated complexes containing six, four, three, two or one solvent molecules were obtained by successive removal of the solvent until in most case the solvent-free metal closo-borates were obtained with the exception of Mg whose hypothetical crystal structure, however, could have its prototype in MnB12H12. The 3d transition metal closo-borates were studied in the view of their potential use as Na- or Li-ion battery electrodes in combination with Na or Li closo-borate solid electrolytes. The metal oxidation state (II) obtained in compounds presented here does not allow such application. View Full-Text
Keywords: Closo-borate; transition metal; ethanol complex; methanol complex; X-ray powder diffraction Closo-borate; transition metal; ethanol complex; methanol complex; X-ray powder diffraction
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Didelot, E.; Łodziana, Z.; Murgia, F.; Černý, R. Ethanol- and Methanol-Coordinated and Solvent-Free Dodecahydro closo-Dodecaborates of 3d Transition Metals and of Magnesium. Crystals 2019, 9, 372.

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