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Non-Mimetic Gels Direct Novel Crystallization Behavior of Lenalidomide [dataset] Open Access

Crystallization within supramolecular gels can yield distinct solid-state outcomes compared to conventional solution-phase methods, including the formation of novel crystal forms or selectively crystallizing one crystal form from a concomitant mixture. In several cases, tailoring the molecular structure of a gelator to mimic a pharmaceutical substrate has facilitated crystallization control, where non-mimetic gelators had no influence on the crystallization outcome compared to the solution phase. In this study, we investigate the crystallization behavior of lenalidomide within both mimetic and non-mimetic gels. Crystallization in a cyclopentanone gel using a non-mimetic gelator led to the discovery of a novel cyclopentanone hemi-solvate, inaccessible via solution-phase crystallization. Additionally, an ethanol gel of the same gelator promoted selective crystallization of the metastable Form 4 in ethanol, in contrast to the thermodynamically favored Form 1 obtained from solution. Gel-phase crystallization using a drug-mimetic gelator produced no deviation from the solution-phase polymorphic outcomes, in contrast to previously reported examples. Solution-state NMR studies showed no evidence of strong interactions between lenalidomide and either gelator, suggesting that the spatial arrangement of the non-mimetic gel fibers and/or possible confinement effects, rather than solution association, plays a critical role in directing crystallization behavior.

Descriptions

Resource type

Dataset

Contributors

Contact person: Steed, Jonathan ¹
Data collector: Steed, Jonathan ¹
Creator: Screen, Martin ¹
Data collector: Screen, Martin ¹
Editor: Screen, Martin ¹

¹ Durham University, UK

Funder

Engineering and Physical Sciences Research Council

Research methods

X-ray Powder Diffraction Rheometry

Other description

Keyword

Gels
Polymorphism
Crystallization
Pharmaceutical

Subject

Colloids--Research
Crystallization
Nuclear magnetic resonance spectroscopy

Location

Language

Cited in

Identifier

ark:/32150/r2tq57nr080
doi:10.15128/r2tq57nr080

Rights

Creative Commons Attribution 4.0 International (CC BY)

Publisher

Durham University

Date Created

File Details

Depositor

J.W. Steed

Date Uploaded

1 July 2025, 10:07:44

Date Modified

2 July 2025, 14:07:35

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Characterization

File format: zip (ZIP Format)

Mime type: application/zip

File size: 40162951

Last modified: 2025:07:01 11:47:55+01:00

Filename: Underlying data for Non-Mimetic Gels Direct Novel Crystallization Behavior of Lenalidomide.zip

Original checksum: 24ae0346e99cf66d2f96827bc9c59837