Structure of Pigment Yellow 181 dimethylsulfoxide N-methyl-2-pyrrolidone (1:1:1) solvate from XRPD plus DFT-D
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With only a 2.6 Å resolution laboratory powder diffraction pattern of the [theta] 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 [theta] 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.
Originalsprog | Engelsk |
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Tidsskrift | Acta Crystallographica. Section B: Structural Science |
Vol/bind | 71 |
Udgave nummer | 1 |
Sider (fra-til) | 89-94 |
Antal sider | 6 |
ISSN | 0108-7681 |
DOI | |
Status | Udgivet - feb. 2015 |
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