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Combining X-ray and NMR crystallography to explore the crystallographic disorder in salbutamol oxalate

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Al-Ani, Aneesa J., Szell, Patrick M. J., Rehman, Zainab, Blade, Helen, Wheatcroft, Helen P., Hughes, Leslie P., Brown, Steven P. and Wilson, Chick C. (2022) Combining X-ray and NMR crystallography to explore the crystallographic disorder in salbutamol oxalate. Crystal Growth & Design, 22 (8). pp. 4696-4707. doi:10.1021/acs.cgd.1c01093 ISSN 1528-7483.

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Official URL: https://doi.org/10.1021/acs.cgd.1c01093

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Abstract

Salbutamol is an active pharmaceutical ingredient commonly used to treat respiratory distress, and is listed by the World Health Organization as an essential medicine. Here, we establish the crystal structure of its oxalate form, salbutamol oxalate, and explore the nature of its crystallographic disorder by combined X-ray crystallography and 13 C cross-polarization (CP) magic-angle spinning (MAS) solid-state NMR. The *C-OH chiral center of salbutamol (note that the crystal structures are a racemic mixture of the two enantiomers of salbutamol) is disordered over two positions, and the tert-butyl group is rotating rapidly, as revealed by 13 C solid-state NMR. The impact of crystallisation conditions on the disorder was investigated, finding variations in the occupancy ratio of the *C-OH chiral center between single crystals, and a consistency across samples in the bulk powder. Overall, this work highlights the contrast between investigating crystallographic disorder by X-ray diffraction, solid-state NMR crystallography, and gauge-including projector augmented wave (GIPAW) DFT calculations, with their combined use yielding an improved understanding of the nature of the crystallographic disorder between the local (i.e., as viewed by NMR) and the longer-range periodic (i.e., as viewed by diffraction) scale.

Item Type: Journal Article
Subjects: Q Science > QD Chemistry
Divisions: Faculty of Science, Engineering and Medicine > Science > Physics
Library of Congress Subject Headings (LCSH): Crystallization, Crystallography, Albuterol, Anions, Nuclear magnetic resonance spectroscopy, Crystal growth
Journal or Publication Title: Crystal Growth & Design
Publisher: American Chemical Society
ISSN: 1528-7483
Official Date: 3 August 2022
Dates:
DateEvent
3 August 2022Published
20 July 2022Available
1 July 2022Accepted
Volume: 22
Number: 8
Page Range: pp. 4696-4707
DOI: 10.1021/acs.cgd.1c01093
Status: Peer Reviewed
Publication Status: Published
Reuse Statement (publisher, data, author rights): 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.1c01093
Access rights to Published version: Open Access (Creative Commons)
Date of first compliant deposit: 13 July 2022
Date of first compliant Open Access: 8 August 2022
RIOXX Funder/Project Grant:
Project/Grant IDRIOXX Funder NameFunder ID
KTP11570Innovate UKhttp://dx.doi.org/10.13039/501100006041
KTP11570AstraZeneca (Firm)http://viaf.org/viaf/954162669634455500001
EP/L016354/1[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266
UNSPECIFIED[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266
UNSPECIFIEDPfizer UKhttp://dx.doi.org/10.13039/100009032
EP/T015063/1[EPSRC] Engineering and Physical Sciences Research Councilhttp://dx.doi.org/10.13039/501100000266
EP/T015063/1[BBSRC] Biotechnology and Biological Sciences Research Councilhttp://dx.doi.org/10.13039/501100000268
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