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Successful strategy for high degree of freedom crystal structure determination from powder X-ray diffraction data: a case study for selexipag form I with 38 DOF

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    SYSNO ASEP0507836
    Document TypeJ - Journal Article
    R&D Document TypeJournal Article
    Subsidiary JČlánek ve WOS
    TitleSuccessful strategy for high degree of freedom crystal structure determination from powder X-ray diffraction data: a case study for selexipag form I with 38 DOF
    Author(s) Hušák, M. (CZ)
    Jegorov, A. (CZ)
    Czernek, Jiří (UMCH-V) RID
    Rohlíček, J. (CZ)
    Žižková, S. (CZ)
    Vraspír, P. (CZ)
    Kolesa, P. (CZ)
    Fitch, A. (FR)
    Brus, Jiří (UMCH-V) RID, ORCID
    Source TitleCrystal Growth & Design. - : AMER CHEMICAL SOC - ISSN 1528-7483
    Roč. 19, č. 8 (2019), s. 4625-4631
    Number of pages7 s.
    Languageeng - English
    CountryUS - United States
    Keywordspowder X-ray diffraction ; DFT methods
    Subject RIVCF - Physical ; Theoretical Chemistry
    OECD categoryPhysical chemistry
    R&D ProjectsLTAUSA18011 GA MŠk - Ministry of Education, Youth and Sports (MEYS)
    Method of publishingLimited access
    Institutional supportUMCH-V - RVO:61389013
    UT WOS000480499600047
    EID SCOPUS85070540180
    DOI10.1021/acs.cgd.9b00517
    AnnotationThe determination of crystal structures from powder X-ray diffraction (PXRD) data by using direct-space methods is significantly limited by the degrees of conformational freedom (DOF). This limit currently lies between 30 and 40 DOF. Novel strategies are thus continuously being developed to allow an increase in DOF while keeping computational time reasonable. In our contribution, we demonstrate the solution of the crystal structure of selexipag, a drug for the treatment of pulmonary arterial hypertension (PAH), from PXRD data using synchrotron radiation. With 38 DOF, this structure is one of the most complex organic molecular structures that was actually solved ab initio from powder diffraction data. As the structure solution problem was on the edge of the current methodological possibilities, we applied an advanced strategy using a combination of restraints from the Cambridge Structural Database (CSD), optimized simulated annealing (SA) parameters, and parallel code execution, all complemented by DFT-D calculations and analysis of solid-state NMR (ss-NMR) parameters. Thus, we present here a novel integrated approach that applies several techniques in conjunction to provide otherwise unavailable structural information.
    WorkplaceInstitute of Macromolecular Chemistry
    ContactEva Čechová, cechova@imc.cas.cz ; Tel.: 296 809 358
    Year of Publishing2020
    Electronic addresshttps://pubs.acs.org/doi/10.1021/acs.cgd.9b00517
Number of the records: 1