Na3GaF6 – A crystal chemical and solid state NMR spectroscopic study

David Böhnisch; Stefan Seidel; Christopher Benndorf; Thomas Jansen; Lena Funke; Rolf-Dieter Hoffmann; Lukas Heletta; Juliane Stahl; Dirk Johrendt; Hellmut Eckert; Thomas Jüstel; Rainer Pöttgen

doi:10.1515/zkri-2017-2138

Article

Na₃GaF₆ – A crystal chemical and solid state NMR spectroscopic study

David Böhnisch , Stefan Seidel , Christopher Benndorf , Thomas Jansen , Lena Funke , Rolf-Dieter Hoffmann , Lukas Heletta , Juliane Stahl , Dirk Johrendt , Hellmut Eckert , Thomas Jüstel and Rainer Pöttgen

Published/Copyright: February 19, 2018

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From the journal Zeitschrift für Kristallographie - Crystalline Materials Volume 233 Issue 7

Abstract

Na₃GaF₆ and Na₃GaF₆:Mn⁴⁺ samples were obtained from NaNO₃ and Ga(NO₃)₃·9H₂O in hydrofluoric acid using K₂MnF₆ or NaMnO₄ as manganese sources. The structure of Na₃GaF₆ was studied by single crystal X-ray diffraction at 90, 293, 440 and 500 K, confirming the monoclinic cryolite type structure, space group P2₁/c. The gallium atoms show slightly distorted octahedral coordination by fluorine atoms, similar to the Na1 atoms. Coordination number 8 is observed for Na2. Both sodium sites are clearly distinguished by ²³Na MAS-NMR spectroscopy. Above 400 K the spectra reveal distinct chemical exchange effects, signifying sodium ion hopping between these two sites. At the same time static ¹⁹F NMR spectra indicate pronounced motional narrowing effects in this temperature region. The nearly invariant ⁶⁹Ga MAS-NMR spectra suggest that any reorientational motion involving the GaF₆³⁻ ions (if present) occurs with preservation of the center of mass of these octahedra.

Keywords: crystal structure; elpasolite; fluorido gallate; solid state NMR spectroscopy

Acknowledgments

This work was supported by the Deutsche Forschungsgemeinschaft and Merck KGaA Darmstadt, Germany. L. F. thanks the Stiftung der Deutschen Wirtschaft for a personal scholarship.

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Received: 2017-11-27

Accepted: 2018-1-29

Published Online: 2018-2-19

Published in Print: 2018-7-26

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https://doi.org/10.1515/zkri-2017-2138

Keywords for this article

crystal structure; elpasolite; fluorido gallate; solid state NMR spectroscopy