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Advanced crystallisation methods for small organic molecules

Advanced crystallisation methods for small organic molecules
Advanced crystallisation methods for small organic molecules

Molecular materials based on small organic molecules often require advanced structural analysis, beyond the capability of spectroscopic techniques, to fully characterise them. In such cases, diffraction methods such as single crystal X-ray diffraction (SCXRD), are one of the most powerful tools available to researchers, providing molecular and structural elucidation at atomic level resolution, including absolute stereochemistry. However SCXRD, and related diffraction methods, are heavily dependent on the availability of suitable, high-quality crystals, thus crystallisation often becomes the major bottleneck in preparing samples. Following a summary of classical methods for the crystallisation of small organic molecules, this review will focus on a number of recently developed advanced methods for crystalline material sample preparation for SCXRD. This review will cover two main areas of modern small organic molecule crystallisation, namely the inclusion of molecules within host complexes (e.g., “crystalline sponge” and tetraaryladamantane based inclusion chaperones) and the use of high-throughput crystallisation, employing “under-oil” approaches (e.g., microbatch under-oil and ENaCt). Representative examples have been included for each technique, together with a discussion of their relative advantages and limitations to aid the reader in selecting the most appropriate technique to overcome a specific analytical challenge.

0306-0012
1995-2010
Metherall, J. P.
36fe44a5-1a20-4509-9a8b-d293b0ebd2e6
Carroll, R. C.
94d92c13-aec3-4d94-a7d4-7a4477b1eb64
Coles, S. J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Hall, M. J.
b813c2f9-7a95-4fe1-8968-4cfcee2f87bb
Probert, M. R.
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Metherall, J. P.
36fe44a5-1a20-4509-9a8b-d293b0ebd2e6
Carroll, R. C.
94d92c13-aec3-4d94-a7d4-7a4477b1eb64
Coles, S. J.
3116f58b-c30c-48cf-bdd5-397d1c1fecf8
Hall, M. J.
b813c2f9-7a95-4fe1-8968-4cfcee2f87bb
Probert, M. R.
a86a95c0-5692-4e4c-9279-a02faf70274c

Metherall, J. P., Carroll, R. C., Coles, S. J., Hall, M. J. and Probert, M. R. (2023) Advanced crystallisation methods for small organic molecules. Chemical Society Reviews, 52 (6), 1995-2010. (doi:10.1039/d2cs00697a).

Record type: Review

Abstract

Molecular materials based on small organic molecules often require advanced structural analysis, beyond the capability of spectroscopic techniques, to fully characterise them. In such cases, diffraction methods such as single crystal X-ray diffraction (SCXRD), are one of the most powerful tools available to researchers, providing molecular and structural elucidation at atomic level resolution, including absolute stereochemistry. However SCXRD, and related diffraction methods, are heavily dependent on the availability of suitable, high-quality crystals, thus crystallisation often becomes the major bottleneck in preparing samples. Following a summary of classical methods for the crystallisation of small organic molecules, this review will focus on a number of recently developed advanced methods for crystalline material sample preparation for SCXRD. This review will cover two main areas of modern small organic molecule crystallisation, namely the inclusion of molecules within host complexes (e.g., “crystalline sponge” and tetraaryladamantane based inclusion chaperones) and the use of high-throughput crystallisation, employing “under-oil” approaches (e.g., microbatch under-oil and ENaCt). Representative examples have been included for each technique, together with a discussion of their relative advantages and limitations to aid the reader in selecting the most appropriate technique to overcome a specific analytical challenge.

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Accepted/In Press date: 1 March 2023
Published date: 1 March 2023
Additional Information: Funding Information: Financial support is acknowledged from EPSRC AstraZeneca (2595838) and the EPSRC National Crystallography Service (EP/W02098X/1; EP/W021129/1; EP/T517914/1). Publisher Copyright: © 2023 The Royal Society of Chemistry.

Identifiers

Local EPrints ID: 476151
URI: http://eprints.soton.ac.uk/id/eprint/476151
ISSN: 0306-0012
PURE UUID: 584699f7-314b-47e1-8fe6-f22b1a573437
ORCID for S. J. Coles: ORCID iD orcid.org/0000-0001-8414-9272

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Date deposited: 12 Apr 2023 16:55
Last modified: 06 Jun 2024 01:37

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Contributors

Author: J. P. Metherall
Author: R. C. Carroll
Author: S. J. Coles ORCID iD
Author: M. J. Hall
Author: M. R. Probert

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