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On the preparation and NMR spectroscopic characterization of potassium aluminium tetrahydride KAlH4

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Zibrowius,  Bodo
Service Department Farès (NMR), Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Felderhoff,  Michael
Research Group Felderhoff, Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Citation

Zibrowius, B., & Felderhoff, M. (2019). On the preparation and NMR spectroscopic characterization of potassium aluminium tetrahydride KAlH4. Physical Chemistry Chemical Physics, 21(23), 12576-12584. doi:10.1039/C9CP01059A.


Cite as: https://hdl.handle.net/21.11116/0000-0004-73E5-8
Abstract
Potassium aluminium tetrahydride KAlH4 of high phase purity (space group Pnma (62)) was synthesized via a mechanochemical route. The thus obtained material was studied by 27Al and 39K MAS NMR spectroscopy. For both nuclei precise data for the isotropic chemical shift and the quadrupole coupling at T = 295 K were derived (27Al: δiso = (107.6 ± 0.2) ppm, CQ = (1.29 ± 0.02) MHz and η = 0.64 ± 0.02; 39K: δiso = (6.1 ± 0.2) ppm, CQ = (0.562 ± 0.005) MHz and η = 0.74 ± 0.02). The straightforward NMR spectroscopic approach applied here should also work for other complex aluminium hydrides and for many other materials containing half-integer nuclei experiencing small to medium-sized quadrupole couplings.