Daria Torodii, Jacob Holmes, Pinelopi Moutzouri, Sten O. Nilsson Lill, Manuel Cordova, Arthur C. Pinon, Kristof Grohe, Sebastian Wegner, Okky Dwichandra Putra, Stefan Tommy Norberg, Anette Welinder, Staffan Schantz, Lyndon Emsley
{"title":"Crystal structure determination of Verinurad via proton-detected ultra-fast MAS NMR and machine learning","authors":"Daria Torodii, Jacob Holmes, Pinelopi Moutzouri, Sten O. Nilsson Lill, Manuel Cordova, Arthur C. Pinon, Kristof Grohe, Sebastian Wegner, Okky Dwichandra Putra, Stefan Tommy Norberg, Anette Welinder, Staffan Schantz, Lyndon Emsley","doi":"10.1039/d4fd00076e","DOIUrl":null,"url":null,"abstract":"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 <small><sup>1</sup></small>H resolution improvement at ultra-fast MAS and use solely <small><sup>1</sup></small>H-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 <small><sup>13</sup></small>C-detected experiments, without the need to employ dynamic nuclear polarization.","PeriodicalId":76,"journal":{"name":"Faraday Discussions","volume":"21 1","pages":""},"PeriodicalIF":3.3000,"publicationDate":"2024-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Faraday Discussions","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1039/d4fd00076e","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, PHYSICAL","Score":null,"Total":0}
引用次数: 0
Abstract
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.