Combining solid state NMR, powder X-ray diffraction, and DFT calculations for CsSc3F10 structure determination

Aydar Rakhmatullin; Mathieu Allix; Ilya B. Polovov; Dmitry Maltsev; Andrey V. Chukin; Rinat Bakirov; Catherine Bessada

doi:10.1016/j.jallcom.2019.01.355

Combining solid state NMR, powder X-ray diffraction, and DFT calculations for CsSc₃F₁₀ structure determination

Aydar Rakhmatullin, Mathieu Allix, Ilya B. Polovov, Dmitry Maltsev, Andrey V. Chukin, Rinat Bakirov, Catherine Bessada

Research output: Contribution to journal › Article › peer-review

9 Scopus citations

Abstract

A combination of high field solid-state MAS NMR spectroscopy, X-ray diffraction, and first-principles calculations is used to elucidate the crystalline structure of CsSc₃F₁₀. At room temperature, this phase was found to crystallize in the Pmma (n°51) space group with a = 8.0837(1) Å, b = 7.5764(1) Å, and c = 6.8127(1) Å. The remarkable feature of CsSc₃F₁₀ is an unusual high cesium coordination number of 18. ⁴⁵Sc -¹⁹F D-HMQC NMR method has been employed to investigate the connectivity of scandium with fluorine atoms. NMR parameters were determined using first principle DFT calculations and compared with experimentally obtained data.

Original language	English
Pages (from-to)	1349-1355
Number of pages	7
Journal	Journal of Alloys and Compounds
Volume	787
DOIs	https://doi.org/10.1016/j.jallcom.2019.01.355
State	Published - May 30 2019
Externally published	Yes

Funding

This work was supported by the Ministry of Education and Science of the Russian Federation № 02.G25.31.0210 of 27.04.2016 . Financial support from the TGIR-RMN-THC Fr3050 CNRS for conducting the research is gratefully acknowledged. For the calculations, we thank the “Centre de Calcul Scientifique en region Centre” (Orleans, France). This work was supported by the Ministry of Education and Science of the Russian Federation №02.G25.31.0210 of 27.04.2016. Financial support from the TGIR-RMN-THC Fr3050 CNRS for conducting the research is gratefully acknowledged. For the calculations, we thank the “Centre de Calcul Scientifique en region Centre” (Orleans, France).

Keywords

CASTEP
Coordination number
Solid-state NMR
X-ray

Access to Document

10.1016/j.jallcom.2019.01.355

Cite this

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title = "Combining solid state NMR, powder X-ray diffraction, and DFT calculations for CsSc3F10 structure determination",

abstract = "A combination of high field solid-state MAS NMR spectroscopy, X-ray diffraction, and first-principles calculations is used to elucidate the crystalline structure of CsSc3F10. At room temperature, this phase was found to crystallize in the Pmma (n°51) space group with a = 8.0837(1) {\AA}, b = 7.5764(1) {\AA}, and c = 6.8127(1) {\AA}. The remarkable feature of CsSc3F10 is an unusual high cesium coordination number of 18. 45Sc -19F D-HMQC NMR method has been employed to investigate the connectivity of scandium with fluorine atoms. NMR parameters were determined using first principle DFT calculations and compared with experimentally obtained data.",

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author = "Aydar Rakhmatullin and Mathieu Allix and Polovov, {Ilya B.} and Dmitry Maltsev and Chukin, {Andrey V.} and Rinat Bakirov and Catherine Bessada",

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T1 - Combining solid state NMR, powder X-ray diffraction, and DFT calculations for CsSc3F10 structure determination

AU - Rakhmatullin, Aydar

AU - Allix, Mathieu

AU - Polovov, Ilya B.

AU - Maltsev, Dmitry

AU - Chukin, Andrey V.

AU - Bakirov, Rinat

AU - Bessada, Catherine

PY - 2019/5/30

Y1 - 2019/5/30

N2 - A combination of high field solid-state MAS NMR spectroscopy, X-ray diffraction, and first-principles calculations is used to elucidate the crystalline structure of CsSc3F10. At room temperature, this phase was found to crystallize in the Pmma (n°51) space group with a = 8.0837(1) Å, b = 7.5764(1) Å, and c = 6.8127(1) Å. The remarkable feature of CsSc3F10 is an unusual high cesium coordination number of 18. 45Sc -19F D-HMQC NMR method has been employed to investigate the connectivity of scandium with fluorine atoms. NMR parameters were determined using first principle DFT calculations and compared with experimentally obtained data.

AB - A combination of high field solid-state MAS NMR spectroscopy, X-ray diffraction, and first-principles calculations is used to elucidate the crystalline structure of CsSc3F10. At room temperature, this phase was found to crystallize in the Pmma (n°51) space group with a = 8.0837(1) Å, b = 7.5764(1) Å, and c = 6.8127(1) Å. The remarkable feature of CsSc3F10 is an unusual high cesium coordination number of 18. 45Sc -19F D-HMQC NMR method has been employed to investigate the connectivity of scandium with fluorine atoms. NMR parameters were determined using first principle DFT calculations and compared with experimentally obtained data.

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