Crystal structure validation of verinurad via proton-detected ultra-fast MAS NMR and machine learning.
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Torodii D, Holmes JB, Moutzouri P, Nilsson Lill SO, Cordova M, Pinon AC, Grohe K, Wegner S, Putra OD, Norberg S, Welinder A, Schantz S, Emsley L
Faraday Discuss. - (-) - [2024-09-19; online 2024-09-19]
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.
Swedish NMR Centre (SNC) [Technology development]
PubMed 39297322
DOI 10.1039/d4fd00076e
Crossref 10.1039/d4fd00076e