Single-crystal structure determination of nanosized metal–organic frameworks by three-dimensional electron diffraction

材料科学 单晶 电子晶体学 纳米技术 瓶颈 透射电子显微镜 衍射 工作流程 计算机科学 电子衍射 结晶学 化学 物理 光学 数据库 嵌入式系统
作者
Taimin Yang,Tom Willhammar,Hongyi Xu,Xiaodong Zou,Zhehao Huang
出处
期刊:Nature Protocols [Nature Portfolio]
卷期号:17 (10): 2389-2413 被引量:55
标识
DOI:10.1038/s41596-022-00720-8
摘要

Metal-organic frameworks (MOFs) have attracted considerable interest due to their well-defined pore architecture and structural tunability on molecular dimensions. While single-crystal X-ray diffraction (SCXRD) has been widely used to elucidate the structures of MOFs at the atomic scale, the formation of large and well-ordered crystals is still a crucial bottleneck for structure determination. To alleviate this challenge, three-dimensional electron diffraction (3D ED) has been developed for structure determination of nano- (submicron-)sized crystals. Such 3D ED data are collected from each single crystal using transmission electron microscopy. In this protocol, we introduce the entire workflow for structural analysis of MOFs by 3D ED, from sample preparation, data acquisition and data processing to structure determination. We describe methods for crystal screening and handling of crystal agglomerates, which are crucial steps in sample preparation for single-crystal 3D ED data collection. We further present how to set up a transmission electron microscope for 3D ED data acquisition and, more importantly, offer suggestions for the optimization of data acquisition conditions. For data processing, including unit cell and space group determination, and intensity integration, we provide guidelines on how to use electron and X-ray crystallography software to process 3D ED data. Finally, we present structure determination from 3D ED data and discuss the important features associated with 3D ED data that need to be considered. We believe that this protocol provides critical details for implementing and utilizing 3D ED as a structure determination platform for nano- (submicron-)sized MOFs as well as other crystalline materials.
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