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Combined Approach for the Structural Characterization of Alkali Fluoroscandates: Solid-State NMR, Powder X‑ray Diffraction, and Density Functional Theory Calculations
journal contribution
posted on 2018-01-22, 19:59 authored by Aydar Rakhmatullin, Ilya B. Polovov, Dmitry Maltsev, Mathieu Allix, Vladimir Volkovich, Andrey V. Chukin, Miroslav Boča, Catherine BessadaThe
structures of several fluoroscandate compounds are presented here
using a characterization approach combining powder X-ray diffraction
and solid-state NMR. The structure of K5Sc3F14 was fully determined from Rietveld refinement performed
on powder X-ray diffraction data. Moreover, the local structures of
NaScF4, Li3ScF6, KSc2F7, and Na3ScF6 compounds were studied
in detail from solid-state 19F and 45Sc NMR
experiments. The 45Sc chemical shift ranges for six- and
seven-coordinated scandium environments were defined. The 19F chemical shift ranges for bridging and terminal fluorine atoms
were also determined. First-principles calculations of the 19F and 45Sc NMR parameters were carried out using plane-wave
basis sets and periodic boundary conditions (CASTEP), and the results were compared with the experimental data. A good
agreement between the calculated shielding constants and experimental
chemical shifts was obtained. This demonstrates the good potential
of computational methods in spectroscopic assignments of solid-state 45Sc NMR spectroscopy.
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Density Functional Theory Calculations45 Sc chemical shift rangesplane-wave basis setsterminal fluorine atomspowder X-ray diffractionNa 3 ScF 6 compoundsLi 3 ScF 645 Sc NMR spectroscopyCASTEPK 5 Sc 3 F 14powder X-ray diffraction dataseven-coordinated scandium environments19 FKSc 2 F 719 F chemical shift ranges45 Sc NMR parameters45 Sc NMR experiments
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