Structure of pigment yellow 181 dimethylsulfoxide N-methyl-2-pyrrolidone (1:1:1) solvate from XRPD + DFT-D
- With only a 2.6 Å resolution laboratory powder diffraction pattern of the θ phase of Pigment Yellow 181 (P.Y. 181) available, crystal-structure solution and Rietveld refinement proved challenging; especially when the crystal structure was shown to be a triclinic dimethylsulfoxide N-methyl-2-pyrrolidone (1:1:1) solvate. The crystal structure, which in principle has 28 possible degrees of freedom, was determined in three stages by a combination of simulated annealing, partial Rietveld refinement with dummy atoms replacing the solvent molecules and further simulated annealing. The θ phase not being of commercial interest, additional experiments were not economically feasible and additional dispersion-corrected density functional theory (DFT-D) calculations were employed to confirm the correctness of the crystal structure. After the correctness of the structure had been ascertained, the bond lengths and valence angles from the DFT-D minimized crystal structure were fed back into the Rietveld refinement as geometrical restraints (‘polymorph-dependent restraints’) to further improve the details of the crystal structure; the positions of the H atoms were also taken from the DFT-D calculations. The final crystal structure is a layered structure with an elaborate network of hydrogen bonds.
Author: | Jacco van de StreekORCiD |
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URN: | urn:nbn:de:hebis:30:3-382452 |
DOI: | https://doi.org/10.1107/S2052520615000724 |
ISSN: | 2052-5206 |
Pubmed Id: | https://pubmed.ncbi.nlm.nih.gov/25643720 |
Parent Title (English): | Acta crystallographica section B |
Publisher: | Wiley-Blackwell |
Place of publication: | Oxford |
Document Type: | Article |
Language: | English |
Date of Publication (online): | 2015/02/01 |
Date of first Publication: | 2015/02/01 |
Publishing Institution: | Universitätsbibliothek Johann Christian Senckenberg |
Release Date: | 2015/10/08 |
Tag: | Pigment Yellow 181; X-ray powder diffraction; dispersion-corrected density functional theory |
Volume: | 71 |
Page Number: | 6 |
First Page: | 89 |
Last Page: | 94 |
Note: | Copyright © Jacco van de Streek 2015. This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited. |
HeBIS-PPN: | 371578574 |
Institutes: | Biochemie, Chemie und Pharmazie / Biochemie und Chemie |
Dewey Decimal Classification: | 5 Naturwissenschaften und Mathematik / 54 Chemie / 540 Chemie und zugeordnete Wissenschaften |
Sammlungen: | Universitätspublikationen |
Licence (German): | Creative Commons - Namensnennung 4.0 |