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

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{
  "updated": "2024-09-17T16:10:17.050226+00:00", 
  "metadata": {
    "_oai": {
      "id": "oai:materialscloud.org:2173"
    }, 
    "version": 1, 
    "is_last": true, 
    "_files": [
      {
        "size": 511034766, 
        "checksum": "md5:179369f56a39d2f1c32c8a98e9d18047", 
        "key": "verinurad_TopSpin_data.zip", 
        "description": "Raw NMR data of the experimental spectra measured."
      }, 
      {
        "size": 3470830, 
        "checksum": "md5:e4b7342c4f2caddd1a98a8ffeaf4f69a", 
        "key": "verinurad_pip_TopSpin_data.zip", 
        "description": "Raw NMR data of the experimental spectra measured and used as input for PIPNet."
      }, 
      {
        "size": 1058281, 
        "checksum": "md5:11db59eb753daa27c3522025da5f8e1a", 
        "key": "Probabilistic_assignment.zip", 
        "description": "The input files used for the Bayesian probabilistic assignment and the complete output data generated"
      }, 
      {
        "size": 28026, 
        "checksum": "md5:b3bd8089ea7d0eb8b31a1d5a32656ce3", 
        "key": "ShiftML2_predictions.zip", 
        "description": "SXRD structure of verinurad with proton relaxed positions used as input for ShiftML2 and the Excel sheet showing the chemical shielding to chemical shift conversion"
      }, 
      {
        "size": 416390, 
        "checksum": "md5:2ec088fd922d934d39462c55dfc47b33", 
        "key": "GIPAW_calculations.zip", 
        "description": "Input/output files for proton optimization and NMR calculation"
      }
    ], 
    "keywords": [
      "Solid-State NMR", 
      "NMR crystallography", 
      "Verinurad"
    ], 
    "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.", 
    "contributors": [
      {
        "affiliations": [
          "Institut des Sciences et Ing\u00e9nierie Chimiques, \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland"
        ], 
        "givennames": "Daria", 
        "email": "daria.torodii@epfl.ch", 
        "familyname": "Torodii"
      }, 
      {
        "affiliations": [
          "Institut des Sciences et Ing\u00e9nierie Chimiques, \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland", 
          "National Centre for Computational Design and Discovery of Novel Materials MARVEL, \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), Lausanne, Switzerland"
        ], 
        "givennames": "Jacob", 
        "familyname": "Holmes"
      }, 
      {
        "affiliations": [
          "Institut des Sciences et Ing\u00e9nierie Chimiques, \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland"
        ], 
        "givennames": "Pinelopi", 
        "familyname": "Moutzouri"
      }, 
      {
        "affiliations": [
          "Data Science & Modelling, Pharmaceutical Sciences, R&D, AstraZeneca, 43183 Gothenburg, Sweden"
        ], 
        "givennames": "Sten", 
        "familyname": "Nilsson Lill"
      }, 
      {
        "affiliations": [
          "Institut des Sciences et Ing\u00e9nierie Chimiques, \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland", 
          "National Centre for Computational Design and Discovery of Novel Materials MARVEL, \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), Lausanne, Switzerland"
        ], 
        "givennames": "Manuel", 
        "familyname": "Cordova"
      }, 
      {
        "affiliations": [
          "Swedish NMR Center, Department of Chemistry and Molecular Biology, University of Gothenburg, 41390 Gothenburg, Sweden"
        ], 
        "givennames": "Arthur", 
        "familyname": "Pinon"
      }, 
      {
        "affiliations": [
          "Bruker BioSpin GmbH & Co KG, 76275 Ettlingen, Germany"
        ], 
        "givennames": "Kristof", 
        "familyname": "Grohe"
      }, 
      {
        "affiliations": [
          "Bruker BioSpin GmbH & Co KG, 76275 Ettlingen, Germany"
        ], 
        "givennames": "Sebastian", 
        "familyname": "Wegner"
      }, 
      {
        "affiliations": [
          "Early Product Development and Manufacturing, Pharmaceutical Sciences, R&D, AstraZeneca, 43183 Gothenburg, Sweden"
        ], 
        "givennames": "Okky Dwichandra", 
        "familyname": "Putra"
      }, 
      {
        "affiliations": [
          "Oral Product Development, Pharmaceutical Technology & Development, Operations, AstraZeneca, 43183 Gothenburg, Sweden"
        ], 
        "givennames": "Stefan", 
        "familyname": "Norberg"
      }, 
      {
        "affiliations": [
          "Oral Product Development, Pharmaceutical Technology & Development, Operations, AstraZeneca, 43183 Gothenburg, Sweden"
        ], 
        "givennames": "Anette", 
        "familyname": "Welinder"
      }, 
      {
        "affiliations": [
          "Oral Product Development, Pharmaceutical Technology & Development, Operations, AstraZeneca, 43183 Gothenburg, Sweden"
        ], 
        "givennames": "Staffan", 
        "familyname": "Schantz"
      }, 
      {
        "affiliations": [
          "Institut des Sciences et Ing\u00e9nierie Chimiques, \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland", 
          "National Centre for Computational Design and Discovery of Novel Materials MARVEL, \u00c9cole Polytechnique F\u00e9d\u00e9rale de Lausanne (EPFL), Lausanne, Switzerland"
        ], 
        "givennames": "Lyndon", 
        "email": "lyndon.emsley@epfl.ch", 
        "familyname": "Emsley"
      }
    ], 
    "edited_by": 576, 
    "owner": 1355, 
    "doi": "10.24435/materialscloud:qk-x9", 
    "title": "Crystal structure validation of verinurad via proton-detected ultra-fast MAS NMR and machine learning", 
    "license": "Creative Commons Attribution 4.0 International", 
    "mcid": "2024.136", 
    "id": "2173", 
    "conceptrecid": "2172", 
    "status": "published", 
    "publication_date": "Sep 17, 2024, 18:10:17", 
    "license_addendum": null, 
    "references": [
      {
        "comment": "Paper with published SXRD structure of verinurad", 
        "type": "Journal reference", 
        "doi": "https://doi.org/10.1021/acs.oprd.1c00284", 
        "citation": "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)"
      }
    ]
  }, 
  "id": "2173", 
  "revision": 4, 
  "created": "2024-05-06T16:34:05.295959+00:00"
}