Accurate structure models and absolute configuration determination using dynamical effects in continuous-rotation 3D electron diffraction data

Research output: Contribution to journalArticleResearchpeer review

Authors

  • Paul B. Klar
  • Yaşar Krysiak
  • Hongyi Xu
  • Gwladys Steciuk
  • Jung Cho
  • Xiaodong Zou
  • Lukas Palatinus

Research Organisations

External Research Organisations

  • Czech Academy of Sciences
  • University of Bremen
  • Stockholm University
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Details

Original languageEnglish
Pages (from-to)848-855
Number of pages8
JournalNature chemistry
Volume15
Issue number6
Early online date20 Apr 2023
Publication statusPublished - Jun 2023

Abstract

Continuous-rotation 3D electron diffraction methods are increasingly popular for the structure analysis of very small organic molecular crystals and crystalline inorganic materials. Dynamical diffraction effects cause non-linear deviations from kinematical intensities that present issues in structure analysis. Here, a method for structure analysis of continuous-rotation 3D electron diffraction data is presented that takes multiple scattering effects into account. Dynamical and kinematical refinements of 12 compounds—ranging from small organic compounds to metal–organic frameworks to inorganic materials—are compared, for which the new approach yields significantly improved models in terms of accuracy and reliability with up to fourfold reduction of the noise level in difference Fourier maps. The intrinsic sensitivity of dynamical diffraction to the absolute structure is also used to assign the handedness of 58 crystals of 9 different chiral compounds, showing that 3D electron diffraction is a reliable tool for the routine determination of absolute structures. [Figure not available: see fulltext.].

Cite this

Accurate structure models and absolute configuration determination using dynamical effects in continuous-rotation 3D electron diffraction data. / Klar, Paul B.; Krysiak, Yaşar; Xu, Hongyi et al.
In: Nature chemistry, Vol. 15, No. 6, 06.2023, p. 848-855.

Research output: Contribution to journalArticleResearchpeer review

Klar PB, Krysiak Y, Xu H, Steciuk G, Cho J, Zou X et al. Accurate structure models and absolute configuration determination using dynamical effects in continuous-rotation 3D electron diffraction data. Nature chemistry. 2023 Jun;15(6):848-855. Epub 2023 Apr 20. doi: 10.1038/s41557-023-01186-1
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title = "Accurate structure models and absolute configuration determination using dynamical effects in continuous-rotation 3D electron diffraction data",
abstract = "Continuous-rotation 3D electron diffraction methods are increasingly popular for the structure analysis of very small organic molecular crystals and crystalline inorganic materials. Dynamical diffraction effects cause non-linear deviations from kinematical intensities that present issues in structure analysis. Here, a method for structure analysis of continuous-rotation 3D electron diffraction data is presented that takes multiple scattering effects into account. Dynamical and kinematical refinements of 12 compounds—ranging from small organic compounds to metal–organic frameworks to inorganic materials—are compared, for which the new approach yields significantly improved models in terms of accuracy and reliability with up to fourfold reduction of the noise level in difference Fourier maps. The intrinsic sensitivity of dynamical diffraction to the absolute structure is also used to assign the handedness of 58 crystals of 9 different chiral compounds, showing that 3D electron diffraction is a reliable tool for the routine determination of absolute structures. [Figure not available: see fulltext.].",
author = "Klar, {Paul B.} and Ya{\c s}ar Krysiak and Hongyi Xu and Gwladys Steciuk and Jung Cho and Xiaodong Zou and Lukas Palatinus",
note = "Funding Information: We thank T. Gr{\"u}ne, J. Wennmacher, J. Bruhn, C. G. Jones, H. M. Nelson, E. Thompson, H. Jenkins, H. Yanagisawa and K. Yamashita for sharing their diffraction data and support with the data formats. Samples of quartz provided by F. Turci (University of Turin) and of abiraterone acetate provided by M. Babor (Zentiva) are highly appreciated. We thank Y. Luo (Stockholm university) for checking the mordenite sample by infrared spectroscopy. We acknowledge the assistance of T. Gr{\"u}ne (University of Vienna), J. P. Abrahams, E. van Genderen (Paul Scherrer Institute) and E. Maddox (Amsterdam Scientific) in understanding the confusion around the determination of absolute structure of epicorazine A and dehydrocurvularin. We are grateful to T. Wagner and P. Piechon (Novartis) for confirming the absolute structure of epicorazine A and dehydrocurvularin by single-crystal XRD. We thank H. Jenkins for indicating a conversion problem with one of the data sets we shared. The work was supported by the Knut and Alice Wallenberg Foundation, grant numbers 2012.0112 and 2018.0237 (X.Z.) and Czech Science Foundation, grant numbers 19-08032S (P.B.K., L.P.) and 21-05926X (G.S., L.P.). G.S., P.B.K. and L.P. acknowledge the CzechNanoLab Research Infrastructure supported by MEYS CR (LM2018110) and the support of the Operational Programme Research, Development and Education financed by European Structural and Investment Funds and MEYS CR (project number SOLID21 CZ.02.1.01/0.0/0.0/16_019/0000760). The funders had no role in study design, data collection and analysis, decision to publish or preparation of the manuscript.",
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T1 - Accurate structure models and absolute configuration determination using dynamical effects in continuous-rotation 3D electron diffraction data

AU - Klar, Paul B.

AU - Krysiak, Yaşar

AU - Xu, Hongyi

AU - Steciuk, Gwladys

AU - Cho, Jung

AU - Zou, Xiaodong

AU - Palatinus, Lukas

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N2 - Continuous-rotation 3D electron diffraction methods are increasingly popular for the structure analysis of very small organic molecular crystals and crystalline inorganic materials. Dynamical diffraction effects cause non-linear deviations from kinematical intensities that present issues in structure analysis. Here, a method for structure analysis of continuous-rotation 3D electron diffraction data is presented that takes multiple scattering effects into account. Dynamical and kinematical refinements of 12 compounds—ranging from small organic compounds to metal–organic frameworks to inorganic materials—are compared, for which the new approach yields significantly improved models in terms of accuracy and reliability with up to fourfold reduction of the noise level in difference Fourier maps. The intrinsic sensitivity of dynamical diffraction to the absolute structure is also used to assign the handedness of 58 crystals of 9 different chiral compounds, showing that 3D electron diffraction is a reliable tool for the routine determination of absolute structures. [Figure not available: see fulltext.].

AB - Continuous-rotation 3D electron diffraction methods are increasingly popular for the structure analysis of very small organic molecular crystals and crystalline inorganic materials. Dynamical diffraction effects cause non-linear deviations from kinematical intensities that present issues in structure analysis. Here, a method for structure analysis of continuous-rotation 3D electron diffraction data is presented that takes multiple scattering effects into account. Dynamical and kinematical refinements of 12 compounds—ranging from small organic compounds to metal–organic frameworks to inorganic materials—are compared, for which the new approach yields significantly improved models in terms of accuracy and reliability with up to fourfold reduction of the noise level in difference Fourier maps. The intrinsic sensitivity of dynamical diffraction to the absolute structure is also used to assign the handedness of 58 crystals of 9 different chiral compounds, showing that 3D electron diffraction is a reliable tool for the routine determination of absolute structures. [Figure not available: see fulltext.].

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