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Single-crystal structure determination of nanosized metal-organic frameworks by three-dimensional electron
Taimin Yang1, Tom Willhammar1, Hongyi Xu2
1Department of Materials and Environmental Chemistry, Stockholm University, Stockholm, Sweden.
Nature Protocols
|July 27, 2022
Summary
Three-dimensional electron diffraction (3D ED) enables atomic-scale structure determination for nano-sized metal-organic frameworks (MOFs). This protocol details the workflow for 3D ED, overcoming crystal size limitations in traditional methods.
Area of Science:
- Materials Science
- Crystallography
- Chemistry
Background:
- Metal-organic frameworks (MOFs) exhibit tunable structures and pore architectures, making them attractive for various applications.
- Single-crystal X-ray diffraction (SCXRD) is limited by the need for large, well-ordered crystals, a common bottleneck in MOF structure determination.
- Nano-sized crystalline materials often cannot be analyzed using conventional SCXRD techniques.
Purpose of the Study:
- To present a comprehensive protocol for structural analysis of MOFs using three-dimensional electron diffraction (3D ED).
- To demonstrate 3D ED as a viable alternative for determining the atomic-scale structures of nano- (submicron-)sized MOF crystals.
- To provide detailed guidelines for implementing 3D ED, from sample preparation to structure determination.
Main Methods:
- Sample preparation techniques, including crystal screening and handling of agglomerates for single-crystal 3D ED.
- Transmission electron microscopy (TEM) setup and optimization for 3D ED data acquisition.
- Data processing using specialized software for unit cell determination, space group assignment, and intensity integration of 3D ED data.
Main Results:
- Successful application of 3D ED for atomic-scale structure determination of nano-sized MOF crystals.
- Detailed workflow encompassing sample preparation, data collection, processing, and structure solution from 3D ED data.
- Identification of key considerations and features specific to 3D ED data analysis.
Conclusions:
- Three-dimensional electron diffraction (3D ED) effectively overcomes the crystal size limitations of SCXRD for MOF structure determination.
- The presented protocol provides a robust framework for utilizing 3D ED for nano- (submicron-)sized crystalline materials.
- 3D ED is established as a powerful platform for atomic-scale structural elucidation of MOFs and other crystalline substances.
