Plana-Ruiz Sergi, Lu Penghan, Ummethala Govind, Dunin-Borkowski Rafal E
Servei de Recursos Científics i Tècnics Universitat Rovira i Virgili Avinguda Països Catalans 26 Tarragona Catalonia43007 Spain.
LENS-MIND, Department of Electronics and Biomedical Engineering Universitat de Barcelona Martí i Franquès 1 Barcelona Catalonia08028 Spain.
J Appl Crystallogr. 2025 Jul 25;58(Pt 4):1249-1260. doi: 10.1107/S1600576725005606. eCollection 2025 Aug 1.
During the past few years, serial electron crystallography (serial electron diffraction) has been gaining attention for the structure determination of crystalline compounds that are sensitive to irradiation by an electron beam. By recording a single electron diffraction pattern per crystal, indexing thousands to tens of thousands of such patterns and merging the reflection intensities of the successfully indexed patterns, one can retrieve crystal structure models with strongly mitigated beam damage contributions. However, one of the technique's bottlenecks is the need to obtain so many well indexed diffraction patterns, which leads to the collection of raw diffraction data in an automated way that usually yields low indexing rates. This work demonstrates how to overcome this limitation by performing the serial crystallography experiment following a semi-automated routine with a precessed electron beam (serial precession electron diffraction). The precession movement increases the number of reflections present in the diffraction patterns, and dynamical effects related to specific orientations of the crystals with respect to the electron beam are greatly minimized. This leads to more uniform reflection intensities across the serial data set, and a smaller number of patterns are required to merge the reflection intensities for good statistics. Furthermore, structure refinements based on the dynamical diffraction theory become possible due to the diffraction volume integration of beam precession, providing a novel approach for more accurate structure models. In this context, the use of beam precession is presented as an advantageous tool for serial electron crystallography, as it enables reliable crystal structure analysis with a lower amount of diffraction data.
在过去几年中,连续电子晶体学(连续电子衍射)在对电子束辐照敏感的晶体化合物的结构测定方面受到了关注。通过记录每个晶体的单个电子衍射图样,对数千到数万个这样的图样进行指标化,并合并成功指标化图样的反射强度,可以获得受束流损伤影响大大减轻的晶体结构模型。然而,该技术的瓶颈之一是需要获得如此多指标良好的衍射图样,这导致以自动化方式收集原始衍射数据,而这通常会产生较低的指标化率。这项工作展示了如何通过采用带倾斜电子束的半自动程序进行连续晶体学实验(连续倾斜电子衍射)来克服这一限制。倾斜运动增加了衍射图样中存在的反射数量,并且与晶体相对于电子束的特定取向相关的动力学效应被大大最小化。这导致在整个连续数据集中反射强度更加均匀,并且合并反射强度以获得良好统计数据所需的图样数量更少。此外,由于束流倾斜的衍射体积积分,基于动力学衍射理论的结构精修成为可能,为获得更精确的结构模型提供了一种新方法。在这种情况下,束流倾斜的使用被视为连续电子晶体学的一种有利工具,因为它能够以较少的衍射数据进行可靠的晶体结构分析。