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Improving confidence in crystal structure solutions using NMR crystallography : the case of β-piroxicam
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Tatton, Andrew S., Blade, Helen, Brown, Steven P., Hodgkinson, Paul, Hughes, Leslie P., Nilsson Lill, Sten and Yates, Jonathan R. (2018) Improving confidence in crystal structure solutions using NMR crystallography : the case of β-piroxicam. Crystal Growth & Design, 18 (6). pp. 3339-3351. doi:10.1021/acs.cgd.8b00022 ISSN 1528-7483.
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WRAP-improving-confidence-crystal-structure-solutions-NMR-crystallography-Brown-2018 .pdf - Accepted Version - Requires a PDF viewer. Download (1489Kb) | Preview |
Official URL: http://dx.doi.org/10.1021/acs.cgd.8b00022
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 optimisation 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.
Item Type: | Journal Article | ||||||||
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | ||||||||
Journal or Publication Title: | Crystal Growth & Design | ||||||||
Publisher: | American Chemical Society | ||||||||
ISSN: | 1528-7483 | ||||||||
Official Date: | 6 June 2018 | ||||||||
Dates: |
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Volume: | 18 | ||||||||
Number: | 6 | ||||||||
Page Range: | pp. 3339-3351 | ||||||||
DOI: | 10.1021/acs.cgd.8b00022 | ||||||||
Status: | Peer Reviewed | ||||||||
Publication Status: | Published | ||||||||
Access rights to Published version: | Restricted or Subscription Access | ||||||||
Date of first compliant deposit: | 20 April 2018 | ||||||||
Date of first compliant Open Access: | 10 April 2019 | ||||||||
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