期刊
JOURNAL OF APPLIED CRYSTALLOGRAPHY
卷 48, 期 -, 页码 718-727出版社
WILEY-BLACKWELL
DOI: 10.1107/S1600576715004604
关键词
electron diffraction tomography; structure solution; precession electron diffraction; direct methods; electron diffraction
A fast and fully automatic procedure for collecting electron diffraction tomography data is presented. In the case of a very stable goniometer it is demonstrated how, by variation of the tilting speed and the CCD detector parameters, it is possible to obtain fully automatic precession-assisted electron diffraction tomography data collections, rotation electron diffraction tomography data collections or new integrated electron diffraction tomography data collections, in which the missing wedge of the reciprocal space between the patterns is recorded by longer exposures during the crystal tilt. It is shown how automatic data collection of limited tilt range can be used to determine the unit-cell parameters, while data of larger tilt range are suitable to solve the crystal structure ab initio with direct methods. The crystal structure of monoclinic MgMoO4 has been solved in this way as a test structure. In the case where the goniometer is not stable enough to guarantee a steady position of the crystal over large tilt ranges, an automatic method for tracking the crystal during continuous rotation of the sample is proposed.
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