University of Oulu

M. Selent, J. Nyman, J. Roukala, M. Ilczyszyn, R. Oilunkaniemi, P. J. Bygrave, R. Laitinen, J. Jokisaari, G. M. Day, P. Lantto, Chem. Eur. J. 2017, 23, 5258. DOI: 10.1002/chem.201604797

Clathrate structure determination by combining crystal structure prediction with computational and experimental ¹²⁹Xe NMR spectroscopy

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Author: Selent, Marcin1,2; Nyman, Jonas3; Roukala, Juho1;
Organizations: 1NMR Research Unit, Faculty of Science, University of Oulu
2Faculty of Chemistry, Wrocław University
3Computational Systems Chemistry, School of Chemistry, University of Southampton
4Laboratory of Inorganic Chemistry, University of Oulu
Format: article
Version: published version
Access: open
Online Access: PDF Full Text (PDF, 1.7 MB)
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Language: English
Published: John Wiley & Sons, 2017
Publish Date: 2018-01-23


We present an approach for the structure determination of clathrates using NMR spectroscopy of enclathrated xenon to select froma set of predicted crystal structures. Crystal structure prediction methods have been used to generate an ensemble of putative structures of o- and m-fluorophenol, whose previously unknown clathrate structures have been studied by ¹²⁹Xe NMR spectroscopy. The high sensitivity of the ¹²⁹Xe chemical shift tensor to the chemical environment and shape of the crystalline cavity makes it ideal as a probe for porous materials. The experimental powder NMR spectra can be used to directly confirm or reject hypothetical crystal structures generated by computational prediction, whose chemical shift tensors have been simulated using density functional theory. For each fluorophenol isomer we find one predicted crystal structure whose measured and computed chemical shift tensors agree within experimental and computational error margins and these are thus proposed as the true fluorophenol xenon clathrate structures.

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Series: Chemistry. A European journal
ISSN: 0947-6539
ISSN-E: 1521-3765
ISSN-L: 0947-6539
Volume: 23
Issue: 22
Pages: 5258 - 5269
DOI: 10.1002/chem.201604797
Type of Publication: A1 Journal article – refereed
Field of Science: 116 Chemical sciences
114 Physical sciences
Funding: The work reported here has been financially supported by the European Research Council under the European Union’s Seventh Framework Programme (FP/2007-2013)/ERC Grant Agreement no. 307358, ERC-stG-2012-ANGLE(J.N.,G.D.), by the Magnus Ehrnrooth Foundation and NGS-NANO (M.S.), and by the Academy of Finland project no.s. 125316, 218191, 255641, and 285666(P. L.).
Academy of Finland Grant Number: 125316
Detailed Information: 125316 (Academy of Finland Funding decision)
218191 (Academy of Finland Funding decision)
255641 (Academy of Finland Funding decision)
285666 (Academy of Finland Funding decision)
Copyright information: © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA. This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited.