A structure determination protocol based on combined analysis of 3D-ED data, powder XRD data, solid-state NMR data and DFT-D calculations reveals the structure of a new polymorph of L-tyrosine
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Authors
Smalley, Christopher
Hoskynes, Harriet
Hughes, Colan
Johnstone, Duncan
Willhammer, Tom
Young, Mark
Logsdail, Andrew
Harris, Kenneth
Publication Date
2022-05-11Journal Title
Chemical Science
ISSN
2041-6520
Publisher
Royal Society of Chemistry
Type
Article
This Version
AM
Metadata
Show full item recordCitation
Smalley, C., Hoskynes, H., Hughes, C., Johnstone, D., Willhammer, T., Young, M., Pickard, C., et al. (2022). A structure determination protocol based on combined analysis of 3D-ED data, powder XRD data, solid-state NMR data and DFT-D calculations reveals the structure of a new polymorph of L-tyrosine. Chemical Science https://doi.org/10.1039/d1sc06467c
Abstract
We report the crystal structure of a new polymorph of L-tyrosine (denoted the β polymorph), prepared by crystallization from the gas phase following vacuum sublimation. Structure determination was carried out by combined analysis of three-dimensional electron diffraction (3D-ED) data and powder X-ray diffraction (XRD) data. Specifically, 3D-ED data were required for reliable unit cell determination and space group assignment, with structure solution carried out independently from both 3D-ED data and powder XRD data using the direct-space strategy for structure solution implemented using a genetic algorithm. Structure refinement was carried out both from powder XRD data using the Rietveld profile refinement technique and from 3D-ED data. The final refined structure was validated both by periodic DFT-D calculations, which confirm that the structure corresponds to an energy minimum on the energy landscape, and by the fact that the values of isotropic 13C NMR chemical shifts calculated for the crystal structure using DFT-D methodology are in good agreement with the experimental high-resolution solid-state 13C NMR spectrum. Based on DFT-D calculations using the PBE0-MBD method, the β polymorph is meta-stable with respect to the previously reported crystal structure of L-tyrosine (now denoted the α polymorph). Crystal structure prediction calculations using the AIRSS approach suggest that there are three other plausible crystalline polymorphs of L-tyrosine, with higher energy than the α and β polymorphs.
Sponsorship
Engineering and Physical Sciences Research Council (EP/P022596/1)
Engineering and Physical Sciences Research Council (EP/R008779/1)
Identifiers
External DOI: https://doi.org/10.1039/d1sc06467c
This record's URL: https://www.repository.cam.ac.uk/handle/1810/335528
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