Issue 23, 2022

Quantitative reversible one pot interconversion of three crystalline polymorphs by ball mill grinding

Abstract

We demonstrate here using a disulfide system the first example of reversible, selective, and quantitative transformation between three crystalline polymorphs by ball mill grinding. This includes the discovery of a previously unknown polymorph. Each polymorph is reproducibly obtained under well-defined neat or liquid-assisted grinding conditions, revealing subtle control over the apparent thermodynamic stability. We discovered that the presence of a contaminant as low as 1.5% mol mol−1 acting as a template is required to enable all these three polymorph transformations. The relative stabilities of the polymorphs are determined by the sizes of the nanocrystals produced under different conditions and by surface interactions with small amounts of added solvent. For the first time, we show evidence that each of the three polymorphs is obtained with a unique and reproducible crystalline size. This mechanochemical approach gives access to bulk quantities of metastable polymorphs that are inaccessible through recrystallisation.

Graphical abstract: Quantitative reversible one pot interconversion of three crystalline polymorphs by ball mill grinding

Supplementary files

Article information

Article type
Paper
Submitted
20 mar 2022
Accepted
11 may 2022
First published
12 may 2022
This article is Open Access
Creative Commons BY license

CrystEngComm, 2022,24, 4256-4261

Quantitative reversible one pot interconversion of three crystalline polymorphs by ball mill grinding

A. M. Belenguer, G. I. Lampronti, A. A. L. Michalchuk, F. Emmerling and J. K. M. Sanders, CrystEngComm, 2022, 24, 4256 DOI: 10.1039/D2CE00393G

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