Comparative Study of Solvatomorphs of Stryker's Reagent Using MicroED and Quantum Mechanics

Area of Science:

• Inorganic Chemistry
• Crystallography
• Materials Science

Background:

• Determining hydrogen atom positions in metal hydrides is crucial for understanding hydride delivery in chemical reactions.
• Traditional X-ray diffraction methods have limitations in precisely locating hydrogen atoms.
• Microcrystal electron diffraction (microED) offers enhanced sensitivity for hydrogen atom detection.

Purpose of the Study:

• To investigate the structure of Stryker's reagent using microcrystal electron diffraction (microED).
• To improve the accuracy of hydrogen atom position determination through quantum crystallography (QCr) and Hirshfeld atom refinement (HAR).
• To characterize a newly discovered benzene solvate of Stryker's reagent.

Main Methods:

• Microcrystal electron diffraction (microED) was employed to collect diffraction data.
• Quantum crystallography (QCr) with Hirshfeld atom refinement (HAR) was used for accurate structural analysis.
• Topological analysis was performed to understand hydride bonding modes.

Main Results:

• The first microED structure of Stryker's reagent was determined, revealing a new benzene solvate.
• Improved accuracy in hydrogen atom positioning was achieved using HAR.
• Structural analysis of the THF solvate confirmed edge-bridging hydrides.
• The new benzene solvate exhibited a mixed edge- and face-bridging hydride configuration.

Conclusions:

• Microcrystal electron diffraction (microED) combined with quantum crystallography (QCr) is effective for precise hydrogen atom localization in metal hydrides.
• The study identified a novel benzene solvate of Stryker's reagent with unique hydride bonding.
• Findings advance the understanding of structural chemistry in metal hydrides and their reactivity.