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Combining the advantages of powder X-ray diffraction and NMR crystallography in structure determination of the pharmaceutical material cimetidine hydrochloride

Watts, Abigail E., Maruyoshi, K, Hughes, Colan Evan, Brown, S and Harris, Kenneth David Maclean 2016. Combining the advantages of powder X-ray diffraction and NMR crystallography in structure determination of the pharmaceutical material cimetidine hydrochloride. Crystal Growth and Design 16 (4) , pp. 1798-1804. 10.1021/acs.cgd.6b00016

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Abstract

We report the crystal structure of the anhydrous phase of cimetidine hydrochloride, determined directly from powder X-ray diffraction data. The material was prepared by dehydration of the readily obtained monohydrate form of cimetidine hydrochloride, the only form for which a crystal structure has previously been reported. As such, solid-state dehydration processes typically yield the product phase as a microcrystalline powder, and structure determination was carried out directly from powder X-ray diffraction data, using the direct-space genetic algorithm technique for structure solution followed by Rietveld refinement. The structure determined from powder X-ray diffraction was further validated by calculating solid-state 13C NMR data for the crystal structure (using first-principles periodic DFT techniques within the GIPAW approach) and assessing the quality of agreement with the corresponding experimental solid-state 13C CPMAS NMR data. This strategy provides a robust vindication of the correctness of the crystal structure by assessing the quality of agreement of the structure both with experimental powder X-ray diffraction data and with experimental solid-state 13C NMR data.

Item Type: Article
Date Type: Publication
Status: Published
Schools: Advanced Research Computing @ Cardiff (ARCCA)
Chemistry
Subjects: Q Science > QD Chemistry
Publisher: American Chemical Society
ISSN: 1528-7483
Date of First Compliant Deposit: 30 March 2016
Date of Acceptance: March 2016
Last Modified: 16 May 2019 14:04
URI: http://orca.cf.ac.uk/id/eprint/88126

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