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Lookup NU author(s): Andrew Tyler, Ronnie Ragbirsingh, Dr Charlie McMonagleORCiD, Dr Paul Waddell, Dr Sarah Heaps, Dr Michael HallORCiD, Professor Mike ProbertORCiD
This work is licensed under a Creative Commons Attribution 4.0 International License (CC BY 4.0).
Single crystal X-ray diffraction analysis (SCXRD) constitutes a universal approach for the elucidation of molecular structure and the study of crystalline forms. However, the discovery of viable crystallisation conditions remains both experimentally challenging and resource intensive, in time and quantity of analyte(s). We report a robot-assisted, high-throughput method for the crystallisation of organic-soluble small molecules, employing only micrograms of analyte per experiment. This allows hundreds of crystallisation conditions to be screened in parallel, with minimal overall sample requirements. Crystals suitable for SCXRD are grown from nanolitre droplets of a solution of analyte in organic solvent(s), each of which is encapsulated within an inert oil to control the rate of solvent loss. This encapsulated nanodroplet crystallisation methodology can also be used to search for new crystal forms, as exemplified through both our discovery of a new (thirteenth) polymorph of the olanzapine precursor ROY and SCXRD analysis of the “uncrystallisable” agrochemical dithianon.
Author(s): Tyler AR, Ragbirsingh R, McMonagle CJ, Waddell PG, Heaps SE, Steed JW, Thaw P, Hall MJ, Probert MR
Publication type: Article
Publication status: Published
Journal: Chem
Year: 2020
Volume: 6
Issue: 7
Pages: 1755-1765
Print publication date: 09/07/2020
Online publication date: 07/05/2020
Acceptance date: 15/04/2020
Date deposited: 03/07/2020
ISSN (print): 2451-9308
ISSN (electronic): 2451-9294
Publisher: Cell Press
URL: https://doi.org/10.1016/j.chempr.2020.04.009
DOI: 10.1016/j.chempr.2020.04.009
Data Access Statement: https://www.ccdc.cam.ac.uk/structures
Notes: https://www.sciencedirect.com/science/article/pii/S2451929420301777
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