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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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cam.issuedOnline2022-03-30
dc.contributor.authorSmalley, Christopher
dc.contributor.authorHoskynes, Harriet
dc.contributor.authorHughes, Colan
dc.contributor.authorJohnstone, Duncan
dc.contributor.authorWillhammer, Tom
dc.contributor.authorYoung, Mark
dc.contributor.authorPickard, Christopher
dc.contributor.authorLogsdail, Andrew
dc.contributor.authorMidgley, Paul
dc.contributor.authorHarris, Kenneth
dc.contributor.orcidPickard, Christopher [0000-0002-9684-5432]
dc.contributor.orcidMidgley, Paul [0000-0002-6817-458X]
dc.date.accessioned2022-07-04T01:02:38Z
dc.date.available2022-07-04T01:02:38Z
dc.date.issued2022-05-11
dc.date.updated2022-07-04T01:02:38Z
dc.description.abstractWe 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.
dc.identifier.doi10.17863/CAM.86140
dc.identifier.eissn2041-6539
dc.identifier.issn2041-6520
dc.identifier.otherPMC9093151
dc.identifier.other35655549
dc.identifier.urihttps://www.repository.cam.ac.uk/handle/1810/338727
dc.languageeng
dc.language.isoeng
dc.publisherRoyal Society of Chemistry
dc.publisher.urlhttp://dx.doi.org/10.1039/d1sc06467c
dc.rightsAttribution 4.0 International
dc.rights.urihttps://creativecommons.org/licenses/by/4.0/
dc.sourceessn: 2041-6539
dc.sourcenlmid: 101545951
dc.subject3402 Inorganic Chemistry
dc.subject34 Chemical Sciences
dc.titleA 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
dc.typeArticle
dcterms.dateAccepted2022-03-29
prism.endingPage5288
prism.issueIdentifier18
prism.publicationNameChemical Science
prism.startingPage5277
prism.volume13
pubs.funder-project-idEngineering and Physical Sciences Research Council (EP/P022596/1)
pubs.funder-project-idEngineering and Physical Sciences Research Council (EP/R008779/1)
rioxxterms.licenseref.urihttps://creativecommons.org/licenses/by/4.0/
rioxxterms.versionVoR
rioxxterms.versionofrecord10.1039/d1sc06467c

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