Crystal structure validation of verinurad via proton-detected ultra-fast MAS NMR and machine learning

Abstract

The recent development of ultra-fast magic-angle spinning (MAS) (>100 kHz) provides new opportunities for structural characterization in solids. Here, we use NMR crystallography to validate the structure of verinurad, a microcrystalline active pharmaceutical ingredient. To do this, we take advantage of 1H resolution improvement at ultra-fast MAS and use solely 1H-detected experiments and machine learning methods to assign all the experimental proton and carbon chemical shifts. This framework provides a new tool for elucidating chemical information from crystalline samples with limited sample volume and yields remarkably faster acquisition times compared to 13C-detected experiments, without the need to employ dynamic nuclear polarization.

Graphical abstract: Crystal structure validation of verinurad via proton-detected ultra-fast MAS NMR and machine learning

Supplementary files

Article information

Article type
Paper
Submitted
15 4 2024
Accepted
07 5 2024
First published
17 7 2024
This article is Open Access
Creative Commons BY license

Faraday Discuss., 2024, Advance Article

Crystal structure validation of verinurad via proton-detected ultra-fast MAS NMR and machine learning

D. Torodii, J. B. Holmes, P. Moutzouri, S. O. Nilsson Lill, M. Cordova, A. C. Pinon, K. Grohe, S. Wegner, O. D. Putra, S. Norberg, A. Welinder, S. Schantz and L. Emsley, Faraday Discuss., 2024, Advance Article , DOI: 10.1039/D4FD00076E

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