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Issue 16, 2019
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Face indexing and shape analysis of salicylamide crystals grown in different solvents

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Abstract

The effect of solvent on salicylamide's crystal habit was investigated. Crystals grown experimentally in acetone, acetonitrile and methanol matched the attachment energy predicted rectangle plate vacuum habit. However, in ethyl acetate irregular hexagonal plate crystals form. This change in habit was found to be caused by the stunted growth of specific crystal faces during the crystallisation process. Single crystal and powder X-ray diffraction was carried out to rule out the possibility of a new polymorph. Given no new polymorphs were discovered, the changing habit makes face indexing of experimentally grown crystals difficult. A combination of experimental and modelling prediction tools was employed for the face indexing process. The interfacial angle between faces combined with preferred orientation P-XRD was found to be the most accurate and reliable method leading to successful identification of each salicylamide crystal face. The surface chemistry of each face was examined on a molecular level with insights into the possible growth attachment sites being made. It is deduced that ethyl acetate is adsorbed more strongly on the faces, the increased size of which, can explain the shape change.

Graphical abstract: Face indexing and shape analysis of salicylamide crystals grown in different solvents

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Article information


Submitted
10 Jan 2019
Accepted
06 Mar 2019
First published
07 Mar 2019

CrystEngComm, 2019,21, 2648-2659
Article type
Paper

Face indexing and shape analysis of salicylamide crystals grown in different solvents

A. Lynch, V. Verma, J. Zeglinski, P. Bannigan and Å. Rasmuson, CrystEngComm, 2019, 21, 2648
DOI: 10.1039/C9CE00049F

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