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
The result's identifiers
Result code in IS VaVaI
<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F61389013%3A_____%2F19%3A00507836" target="_blank" >RIV/61389013:_____/19:00507836 - isvavai.cz</a>
Alternative codes found
RIV/60461373:22310/19:43918684
Result on the web
<a href="https://pubs.acs.org/doi/10.1021/acs.cgd.9b00517" target="_blank" >https://pubs.acs.org/doi/10.1021/acs.cgd.9b00517</a>
DOI - Digital Object Identifier
<a href="http://dx.doi.org/10.1021/acs.cgd.9b00517" target="_blank" >10.1021/acs.cgd.9b00517</a>
Alternative languages
Result language
angličtina
Original language name
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
Original language description
The 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.
Czech name
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Czech description
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Classification
Type
J<sub>imp</sub> - Article in a specialist periodical, which is included in the Web of Science database
CEP classification
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OECD FORD branch
10403 - Physical chemistry
Result continuities
Project
<a href="/en/project/LTAUSA18011" target="_blank" >LTAUSA18011: Ab Initio Investigation of Polymorphism of Active Pharmaceutical Ingredients Supported by State of the Art NMR Crystallographic and Calorimetric Experiments.</a><br>
Continuities
P - Projekt vyzkumu a vyvoje financovany z verejnych zdroju (s odkazem do CEP)
Others
Publication year
2019
Confidentiality
S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů
Data specific for result type
Name of the periodical
Crystal Growth & Design
ISSN
1528-7483
e-ISSN
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Volume of the periodical
19
Issue of the periodical within the volume
8
Country of publishing house
US - UNITED STATES
Number of pages
7
Pages from-to
4625-4631
UT code for WoS article
000480499600047
EID of the result in the Scopus database
2-s2.0-85070540180