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materialscloud:2024.136
Published September 17, 2024 | Version v1
Dataset Open

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

Creators

  • 1. Institut des Sciences et Ingénierie Chimiques, École Polytechnique Fédérale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland
  • 2. National Centre for Computational Design and Discovery of Novel Materials MARVEL, École Polytechnique Fédérale de Lausanne (EPFL), Lausanne, Switzerland
  • 3. Data Science & Modelling, Pharmaceutical Sciences, R&D, AstraZeneca, 43183 Gothenburg, Sweden
  • 4. Swedish NMR Center, Department of Chemistry and Molecular Biology, University of Gothenburg, 41390 Gothenburg, Sweden
  • 5. Bruker BioSpin GmbH & Co KG, 76275 Ettlingen, Germany
  • 6. Early Product Development and Manufacturing, Pharmaceutical Sciences, R&D, AstraZeneca, 43183 Gothenburg, Sweden
  • 7. Oral Product Development, Pharmaceutical Technology & Development, Operations, AstraZeneca, 43183 Gothenburg, Sweden

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Description

The recent development of ultra-fast 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.

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References

Journal reference (Paper with published SXRD structure of verinurad)
O. T. Ring, B. R. Hayter, T. O. Ronson, L. R. Agnew, I. W. Ashworth, J. Cherryman, M. A. Y. Gall, P. R. Hamilton, P. A. Inglesby, M. F. Jones, A. L. Lamacraft, A. J. Leahy, D. McKinney, L. Miller-Potucka, L. Powell, O. D. Putra, A. J. Robbins, S. Tomasi and R. A. Wordsworth, Organic Process Research & Development 26, 936-948 (2022), doi: 10.1021/acs.oprd.1c00284

Journal reference (External reference to the paper)
D. Torodii, J. Holmes, P. Moutzouri, S. Nilsson Lill, M. Cordova, A. Pinon, K. Grohe, S. Wegner, O. Putra, S. Norberg, A. Welinder, S. Schantz, L. Emsley, Faraday Discussion 225, 143-158, 2025, doi: 10.1039/d4fd00076e

Journal reference (External reference to the paper)
D. Torodii, J. Holmes, P. Moutzouri, S. Nilsson Lill, M. Cordova, A. Pinon, K. Grohe, S. Wegner, O. Putra, S. Norberg, A. Welinder, S. Schantz, L. Emsley, Faraday Discussion 225, 143-158, 2025