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

Ana M. Belenguer; Giulio I. Lampronti; Adam A. L. Michalchuk; Franziska Emmerling; Jeremy K. M. Sanders

doi:10.1039/d2ce00393g

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

Ana M. Belenguer, Giulio I. Lampronti, Adam A. L. Michalchuk, Franziska Emmerling, Jeremy K. M. Sanders

Chemistry

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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.

Original language	English
Pages (from-to)	4256-4261
Number of pages	6
Journal	CrystEngComm
Volume	24
Issue number	23
Early online date	12 May 2022
DOIs	https://doi.org/10.1039/d2ce00393g
Publication status	Published - 21 Jun 2022

Bibliographical note

Funding Information:
Experiments were conducted at the Yusuf Hamied Department of Chemistry and Department of Earth Sciences, University of Cambridge, and at BAM (Federal Institute for Materials Research and Testing) in Berlin. AMB, AALM and FE thank D. Al-Sabbagh for support with PXRD at BAM. In Cambridge Chemistry we thank C. Truscott for support of PXRD, C. A. Bland and P. Donnelly for the mechanical and software design of the automation of the grinders for repeat grinding, the mechanical workshop team for the manufacture of the jars and the Chris Hunter research, for general support. G.I.L. thanks the Department of Earth Sciences for general support. The authors acknowledge COST Action CA18112 - Mechanochemistry for Sustainable Industry.

Publisher Copyright:
© 2022 The Royal Society of Chemistry

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title = "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.",

author = "Belenguer, {Ana M.} and Lampronti, {Giulio I.} and Michalchuk, {Adam A. L.} and Franziska Emmerling and Sanders, {Jeremy K. M.}",

note = "Funding Information: Experiments were conducted at the Yusuf Hamied Department of Chemistry and Department of Earth Sciences, University of Cambridge, and at BAM (Federal Institute for Materials Research and Testing) in Berlin. AMB, AALM and FE thank D. Al-Sabbagh for support with PXRD at BAM. In Cambridge Chemistry we thank C. Truscott for support of PXRD, C. A. Bland and P. Donnelly for the mechanical and software design of the automation of the grinders for repeat grinding, the mechanical workshop team for the manufacture of the jars and the Chris Hunter research, for general support. G.I.L. thanks the Department of Earth Sciences for general support. The authors acknowledge COST Action CA18112 - Mechanochemistry for Sustainable Industry. Publisher Copyright: {\textcopyright} 2022 The Royal Society of Chemistry",

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AU - Lampronti, Giulio I.

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AU - Emmerling, Franziska

AU - Sanders, Jeremy K. M.

N1 - Funding Information: Experiments were conducted at the Yusuf Hamied Department of Chemistry and Department of Earth Sciences, University of Cambridge, and at BAM (Federal Institute for Materials Research and Testing) in Berlin. AMB, AALM and FE thank D. Al-Sabbagh for support with PXRD at BAM. In Cambridge Chemistry we thank C. Truscott for support of PXRD, C. A. Bland and P. Donnelly for the mechanical and software design of the automation of the grinders for repeat grinding, the mechanical workshop team for the manufacture of the jars and the Chris Hunter research, for general support. G.I.L. thanks the Department of Earth Sciences for general support. The authors acknowledge COST Action CA18112 - Mechanochemistry for Sustainable Industry. Publisher Copyright: © 2022 The Royal Society of Chemistry

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N2 - 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.

AB - 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.

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

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