Reactive Noble-Gas Compounds Explored by 3D Electron Diffraction: XeF₂-MnF₄ Adducts and a Facile Sample Handling...

Area of Science:

• Inorganic Chemistry
• Materials Science
• Crystallography

Background:

• Single-crystal X-ray diffraction (SCXRD) is limited by crystal size requirements.
• Main-group chemistry often involves poorly crystalline or difficult-to-grow single crystals.
• Noble-gas compounds present unique challenges due to their reactivity and instability.

Purpose of the Study:

• To develop a facile method for analyzing air-sensitive and oxidizing samples using 3D electron diffraction (3D ED).
• To investigate the structural chemistry of xenon difluoride-metal tetrafluoride adducts.
• To demonstrate the applicability of 3D ED for studying noble-gas compounds and reactive species.

Main Methods:

• Development of a low-temperature loading and transfer technique for transmission electron microscopy (TEM).
• Application of 3D electron diffraction (3D ED) on submicron crystals of xenon compounds.
• Dynamical refinement of 3D ED data and comparison with SCXRD and density-functional theory (DFT) calculations.

Main Results:

• Successfully determined crystal structures of xenon(II) compounds (3XeF₂·2MnF₄, XeF₂·MnF₄, XeF₂·2MnF₄) using 3D ED on nanometer-sized crystallites.
• Structural data from 3D ED were in complete agreement with SCXRD and DFT calculations.
• Established a robust method for handling and analyzing highly reactive and air-sensitive materials.

Conclusions:

• 3D electron diffraction (3D ED) is a powerful technique for structural analysis of main-group compounds, especially those with challenging crystal growth.
• The developed low-temperature method facilitates the study of sensitive noble-gas compounds.
• This work advances the understanding of xenon difluoride-metal tetrafluoride adducts and related reactive systems.