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Reactive Noble-Gas Compounds Explored by 3D Electron Diffraction: XeF2–MnF4 Adducts and a Facile Sample Handling Procedure
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Reactive Noble-Gas Compounds Explored by 3D Electron Diffraction: XeF2–MnF4 Adducts and a Facile Sample Handling Procedure
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  • Klemen Motaln
    Klemen Motaln
    Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia
    Jožef Stefan International Postgraduate School, Jamova cesta 39, 1000 Ljubljana, Slovenia
  • Kshitij Gurung
    Kshitij Gurung
    Department of Structure Analysis, Institute of Physics of the Czech Academy of Sciences, Na Slovance 1999/2, Prague 8, 18221, Czech Republic
  • Petr Brázda
    Petr Brázda
    Department of Structure Analysis, Institute of Physics of the Czech Academy of Sciences, Na Slovance 1999/2, Prague 8, 18221, Czech Republic
    More by Petr Brázda
  • Anton Kokalj
    Anton Kokalj
    Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia
    Jožef Stefan International Postgraduate School, Jamova cesta 39, 1000 Ljubljana, Slovenia
    More by Anton Kokalj
  • Kristian Radan
    Kristian Radan
    Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia
  • Mirela Dragomir
    Mirela Dragomir
    Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia
    Jožef Stefan International Postgraduate School, Jamova cesta 39, 1000 Ljubljana, Slovenia
  • Boris Žemva
    Boris Žemva
    Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia
    Jožef Stefan International Postgraduate School, Jamova cesta 39, 1000 Ljubljana, Slovenia
    More by Boris Žemva
  • Lukáš Palatinus*
    Lukáš Palatinus
    Department of Structure Analysis, Institute of Physics of the Czech Academy of Sciences, Na Slovance 1999/2, Prague 8, 18221, Czech Republic
    *Email: [email protected] (L.P.).
  • Matic Lozinšek*
    Matic Lozinšek
    Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia
    Jožef Stefan International Postgraduate School, Jamova cesta 39, 1000 Ljubljana, Slovenia
    *Email: [email protected] (M.L.).
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ACS Central Science

Cite this: ACS Cent. Sci. 2024, XXXX, XXX, XXX-XXX
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https://doi.org/10.1021/acscentsci.4c00815
Published August 14, 2024

© 2024 The Authors. Published by American Chemical Society. This publication is licensed under

CC-BY 4.0 .

Abstract

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Recent advances in 3D electron diffraction (3D ED) have succeeded in matching the capabilities of single-crystal X-ray diffraction (SCXRD), while requiring only submicron crystals for successful structural investigations. One of the many diverse areas to benefit from the 3D ED structural analysis is main-group chemistry, where compounds are often poorly crystalline or single-crystal growth is challenging. A facile method for loading and transferring highly air-sensitive and strongly oxidizing samples at low temperatures to a transmission electron microscope (TEM) for 3D ED analysis was successfully developed and tested on xenon(II) compounds from the XeF2–MnF4 system. The crystal structures determined on nanometer-sized crystallites by dynamical refinement of the 3D ED data are in complete agreement with the results obtained by SCXRD on micrometer-sized crystals and by periodic density-functional theory (DFT) calculations, demonstrating the applicability of this approach for structural studies of noble-gas compounds and highly reactive species in general. The compounds 3XeF2·2MnF4, XeF2·MnF4, and XeF2·2MnF4 are rare examples of structurally fully characterized xenon difluoride–metal tetrafluoride adducts and thus advance our knowledge of the diverse structural chemistry of these systems, which also includes the hitherto poorly characterized first noble-gas compound, “XePtF6”.

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Supporting Information

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The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acscentsci.4c00815.

  • Detailed descriptions of experimental and computational procedures, PXRD data, additional crystallographic data (Table S13) and figures, IR spectra (Figures S16, S17; Table S14) and visualizations of the calculated vibrational modes (Figure S18–S20), and the DFT-optimized structure coordinates (PDF)

  • Crystallographic information files (CIF) for 3XeF2·2MnF4, XeF2·MnF4, and XeF2·2MnF4, determined by both 3D ED and SCXRD (CSD 2368882–2368887) (ZIP-1 and ZIP-2).

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ACS Central Science

Cite this: ACS Cent. Sci. 2024, XXXX, XXX, XXX-XXX
Click to copy citationCitation copied!
https://doi.org/10.1021/acscentsci.4c00815
Published August 14, 2024

© 2024 The Authors. Published by American Chemical Society. This publication is licensed under

CC-BY 4.0 .

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