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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

SYSNO ASEP	0507836
Document Type	J - Journal Article
R&D Document Type	Journal Article
Subsidiary J	Článek ve WOS
Title	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
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 Title	Crystal Growth & Design. - : American Chemical Society - ISSN 1528-7483 Roč. 19, č. 8 (2019), s. 4625-4631
Number of pages	7 s.
Language	eng - English
Country	US - United States
Keywords	powder X-ray diffraction ; DFT methods
Subject RIV	CF - Physical ; Theoretical Chemistry
OECD category	Physical chemistry
R&D Projects	LTAUSA18011 GA MŠMT - Ministry of Education, Youth and Sports (MEYS)
Method of publishing	Limited access
Institutional support	UMCH-V - RVO:61389013
UT WOS	000480499600047
EID SCOPUS	85070540180
DOI	10.1021/acs.cgd.9b00517
Annotation	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.
Workplace	Institute of Macromolecular Chemistry
Contact	Eva Čechová, cechova@imc.cas.cz ; Tel.: 296 809 358
Year of Publishing	2020
Electronic address	https://pubs.acs.org/doi/10.1021/acs.cgd.9b00517

Number of the records: 1