Improving Confidence in Crystal Structure Solutions Using NMR Crystallography: The Case of β-Piroxicam

Tatton, Andrew S.; Blade, Helen; Brown, Steven P.; Hodgkinson, Paul; Hughes, Leslie P.; Lill, Sten O. Nilsson; Yates, Jonathan R.

doi:10.1021/acs.cgd.8b00022

Improving Confidence in Crystal Structure Solutions Using NMR Crystallography: The Case of β-Piroxicam

Tatton, Andrew S.; Blade, Helen; Brown, Steven P.; Hodgkinson, Paul; Hughes, Leslie P.; Lill, Sten O. Nilsson; Yates, Jonathan R.

Authors

Andrew S. Tatton

Helen Blade

Steven P. Brown

Professor Paul Hodgkinson paul.hodgkinson@durham.ac.uk
Professor

Leslie P. Hughes

Sten O. Nilsson Lill

Jonathan R. Yates

Abstract

NMR crystallographic techniques are used to validate a structure of β-piroxicam determined from powder X-ray diffraction (PXRD) with a relatively poor R-factor. Geometry optimization of PXRD- and single-crystal XRD- derived structures results in convergence to the same energy of the structures, with minimal atomic displacements, and good agreement of gauge-included projector augmented wave (GIPAW) calculated and experimentally determined NMR 1H, 13C, and 15N chemical shifts, and 14N quadrupolar parameters. Calculations on isolated molecules combined with 2D magic-angle spinning (MAS) 1H double-quantum (DQ) and 14N–1H NMR experiments confirm the 3D packing arrangement of β-piroxicam. NMR crystallography is shown to be an effective means of validating crystal structures that might otherwise be considered sceptically on the basis of diffraction data alone.

Citation

Tatton, A. S., Blade, H., Brown, S. P., Hodgkinson, P., Hughes, L. P., Lill, S. O. N., & Yates, J. R. (2018). Improving Confidence in Crystal Structure Solutions Using NMR Crystallography: The Case of β-Piroxicam. Crystal Growth and Design, 18(6), 3339-3351. https://doi.org/10.1021/acs.cgd.8b00022

Journal Article Type	Article
Acceptance Date	Apr 10, 2018
Online Publication Date	Apr 10, 2018
Publication Date	Apr 10, 2018
Deposit Date	Jun 28, 2018
Publicly Available Date	Apr 10, 2019
Journal	Crystal Growth and Design
Print ISSN	1528-7483
Electronic ISSN	1528-7505
Publisher	American Chemical Society
Peer Reviewed	Peer Reviewed
Volume	18
Issue	6
Pages	3339-3351
DOI	https://doi.org/10.1021/acs.cgd.8b00022

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Copyright Statement
This document is the Accepted Manuscript version of a Published Work that appeared in final form in Crystal growth & design, copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see https://doi.org/10.1021/acs.cgd.8b00022