标题： 透射电子显微镜的实用晶体学 显示英文标题

标题： Practical Crystallography with a Transmission Electron Microscope

摘要： 三维电子衍射（3DED）是一种强大的技术，能够提供亚微米大小晶体的晶体结构解决方案，这些晶体太小，无法通过X射线技术进行结构确定。 然而，需要配备专门软件的透射电子显微镜（TEM），以实现样品台的协调旋转和连续电子衍射数据采集，这一要求通常限制了3DED的广泛应用。 为解决这一限制，我们介绍了适用于受控3DED数据采集的新软件GiveMeED。 使用超过0.8 {\AA } 的可用反射收集，使3DED晶体学处理变得切实可行，使用来自单晶X射线衍射（SCXRD）技术的标准软件和工作流程。 在实际术语中描述了在常规TEM上进行3DED的完整实验流程，结合直接成像、能量色散X射线光谱（EDS）和电子能量损失光谱（EELS），以返回对晶体形态和样品组成的全面相关描述，并充分考虑表征过程中每个阶段的电子通量量化。 通过案例研究对乙酰氨基酚、铜(II)酞菁和高氯代冠烯样品的结构解析，展示了GiveMeED的准确性和有效性，在受控低剂量条件下于室温或冷冻温度下以接近天然状态进行表征，确定的晶胞参数和原子连接性与这些化合物的公认文献X射线结构相匹配。 为了促进3DED的更广泛应用，我们免费提供GiveMeED供使用和修改，以支持通过电子衍射进行结构解析程序的更大采用和利用。 显示英文摘要

摘要： Three-dimensional electron diffraction (3DED) is a powerful technique providing for crystal structure solutions of sub-micron sized crystals too small for structure determination via X-ray techniques. The entry requirement, however, of a transmission electron microscope (TEM) adapted with bespoke software for coordinated sample stage rotation and continuous electron diffraction data acquisition has generally inhibited the wider uptake of 3DED. To address this limitation, we present novel software GiveMeED appropriate for controlled 3DED data acquisition. The collection of useable reflections beyond 0.8 {\AA} makes 3DED crystallographic processing effectively routine, using standard software and workflows derived from single-crystal X-ray diffraction (SCXRD) techniques. A full experimental workflow for 3DED on a conventional TEM is described in practical terms, in combination with direct imaging, and energy dispersive X-ray spectroscopy (EDS) and electron energy loss spectroscopy (EELS), for the return of comprehensive correlative descriptions of crystal morphologies and sample compositions, with due regard for the quantification of electron flux at each stage of the characterisation process. The accuracy and effectiveness of GiveMeED is demonstrated through structure solutions for case study paracetamol, copper(II) phthalocyanine, and percholorocoronene samples, characterised in their near-native states under controlled low dose conditions at either room or cryogenic temperatures, with determined unit cell parameters and atomic connectivity matching accepted literature X-ray structures for these compounds. To promote the wider adoption of 3DED, we make GiveMeED freely available for use and modification, in support of greater uptake and utilisation of structure solution procedures via electron diffraction.