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Polymorph identification and crystal structure determination by a combined crystal structure prediction and transmission electron microscopy approach

Polymorph identification and crystal structure determination by a combined crystal structure prediction and transmission electron microscopy approach
Polymorph identification and crystal structure determination by a combined crystal structure prediction and transmission electron microscopy approach
Electron diffraction offers advantages over X-ray based methods for crystal structure determination because it can be applied to sub-micron sized crystallites, and picogram quantities of material. For molecular organic species, however, crystal structure determination with electron diffraction is hindered by rapid crystal deterioration in the electron beam, limiting the amount of diffraction data that can be collected, and by the effect of dynamical scattering on reflection intensities. Automated electron diffraction tomography provides one possible solution. We demonstrate here, however, an alternative approach in which a set of putative crystal structures of the compound of interest is generated by crystal structure prediction methods and electron diffraction is used to determine which of these putative structures is experimentally observed. This approach enables the advantages of electron diffraction to be exploited, while avoiding the need to obtain large amounts of diffraction data or accurate reflection intensities. We demonstrate the application of the methodology to the pharmaceutical compounds paracetamol, scyllo-inositol and theophylline.
analytical methods, computational chemistry, electron diffraction, electron microscopy, structure elucidation
0947-6539
7874-7882
Eddleston, Mark D.
01211ad8-8115-43de-914c-6501d1d4c584
Hejczyk, Katarzyna E.
de9b9785-9e41-4816-a309-982b3347a429
Bithell, Erica G.
b901e038-97a7-4ba4-9081-80274f1ef7f6
Day, Graeme M.
e3be79ba-ad12-4461-b735-74d5c4355636
Jones, William
3173abf0-1cfa-45f0-996e-2586b385c21e
Eddleston, Mark D.
01211ad8-8115-43de-914c-6501d1d4c584
Hejczyk, Katarzyna E.
de9b9785-9e41-4816-a309-982b3347a429
Bithell, Erica G.
b901e038-97a7-4ba4-9081-80274f1ef7f6
Day, Graeme M.
e3be79ba-ad12-4461-b735-74d5c4355636
Jones, William
3173abf0-1cfa-45f0-996e-2586b385c21e

Eddleston, Mark D., Hejczyk, Katarzyna E., Bithell, Erica G., Day, Graeme M. and Jones, William (2013) Polymorph identification and crystal structure determination by a combined crystal structure prediction and transmission electron microscopy approach. Chemistry - A European Journal, 19 (24), 7874-7882. (doi:10.1002/chem.201204368). (PMID:23592444)

Record type: Article

Abstract

Electron diffraction offers advantages over X-ray based methods for crystal structure determination because it can be applied to sub-micron sized crystallites, and picogram quantities of material. For molecular organic species, however, crystal structure determination with electron diffraction is hindered by rapid crystal deterioration in the electron beam, limiting the amount of diffraction data that can be collected, and by the effect of dynamical scattering on reflection intensities. Automated electron diffraction tomography provides one possible solution. We demonstrate here, however, an alternative approach in which a set of putative crystal structures of the compound of interest is generated by crystal structure prediction methods and electron diffraction is used to determine which of these putative structures is experimentally observed. This approach enables the advantages of electron diffraction to be exploited, while avoiding the need to obtain large amounts of diffraction data or accurate reflection intensities. We demonstrate the application of the methodology to the pharmaceutical compounds paracetamol, scyllo-inositol and theophylline.

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e-pub ahead of print date: 16 April 2013
Published date: June 2013
Keywords: analytical methods, computational chemistry, electron diffraction, electron microscopy, structure elucidation
Organisations: Chemistry

Identifiers

Local EPrints ID: 351756
URI: http://eprints.soton.ac.uk/id/eprint/351756
ISSN: 0947-6539
PURE UUID: 0e8239dc-4133-483c-902f-8ecdd44409fc
ORCID for Graeme M. Day: ORCID iD orcid.org/0000-0001-8396-2771

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Date deposited: 30 Apr 2013 12:16
Last modified: 26 Nov 2019 01:37

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