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On the quality of the continuous rotation electron diffraction data for accurate atomic structure determination of inorganic compounds
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).ORCID iD: 0000-0001-6748-6656
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Number of Authors: 52018 (English)In: Journal of applied crystallography, ISSN 0021-8898, E-ISSN 1600-5767, Vol. 51, p. 1094-1101Article in journal (Refereed) Published
Abstract [en]

The continuous rotation electron diffraction (cRED) method has the capability of providing fast three-dimensional electron diffraction data collection on existing and future transmission electron microscopes; unknown structures could be potentially solved and refined using cRED data collected from nano-and submicrometre-sized crystals. However, structure refinements of cRED data using SHELXL often lead to relatively high R1 values when compared with those refined against single-crystal X-ray diffraction data. It is therefore necessary to analyse the quality of the structural models refined against cRED data. In this work, multiple cRED data sets collected from different crystals of an oxofluoride (FeSeO3F) and a zeolite (ZSM-5) with known structures are used to assess the data consistency and quality and, more importantly, the accuracy of the structural models refined against these data sets. An evaluation of the precision and consistency of the cRED data by examination of the statistics obtained from the data processing software DIALS is presented. It is shown that, despite the high R1 values caused by dynamical scattering and other factors, the refined atomic positions obtained from the cRED data collected for different crystals are consistent with those of the reference models refined against single-crystal X-ray diffraction data. The results serve as a reference for the quality of the cRED data and the achievable accuracy of the structural parameters.

Place, publisher, year, edition, pages
2018. Vol. 51, p. 1094-1101
Keywords [en]
electron diffraction, continuous rotation electron diffraction, structure determination, structure refinement, oxofluorides, zeolites
National Category
Chemical Sciences
Research subject
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-158915DOI: 10.1107/S1600576718007604ISI: 000440411700014OAI: oai:DiVA.org:su-158915DiVA, id: diva2:1240018
Available from: 2018-08-20 Created: 2018-08-20 Last updated: 2019-02-13Bibliographically approved
In thesis
1. 3D Electron Microscopy Methods and Applications: Structures from Atomic Scale to Mesoscale
Open this publication in new window or tab >>3D Electron Microscopy Methods and Applications: Structures from Atomic Scale to Mesoscale
2019 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The crystal structure determines the physical properties of a material. The structure can be analysed at different levels, from atomic level, mesoscale level, all the way up to the macroscale level. Transmission Electron Microscope (TEM) is a powerful tool for studying the structure of materials at atomic scale level and mesoscale level because of the short wavelength of the electrons. At atomic scale level, structure determination using TEM can be performed in diffraction mode. The recent developments in 3D electron diffraction methods make structure determination from nano- and micron-sized crystals much easier than before. However, due to the strong interactions, electrons can be scattered multiple times through the crystal, causing the measured intensities to be less accurate than that in the X-ray case.

In this thesis, we use the continuous rotation electron diffraction (cRED) developed in our group to investigate the structure of materials and the accuracy of this method. In the third chapter, we use cRED method to determine the structure of two aluminophosphate zeolites, PST-13 and PST-14. We presented that these structures can be built from two pairs of enantiomeric structural building units. In the fourth chapter, we show that despite the inaccuracy in measured intensities originated from dynamical effect, it is still possible to determine the structure accurately. We show that the atomic coordinates of ZSM-5 and sucrose crystal structure determined by multiple electron diffraction datasets is identical to that determined from X-ray data or neutron data. We also assessed the linearity between calculated structure factor and observed structure factor and use this as a coarse assessment indicator for diffraction data quality for protein crystals.

Apart from atomic structure, mesoscale structures, such as mesopores, can also determine the property of materials. For the 3D structures of these nanoscale structures, we can also use TEM electron tomography techniques to investigate. In chapter five, we performed electron tomography for two different materials with mesoporous structure and illustrated the formation mechanism of mesoporous magnesium carbonate and the internal tunnel structure of hierarchical TS-1 zeolite.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2019. p. 58
Keywords
3D Electron microscopy, continuous rotation electron diffraction, structure determination, data quality, electron tomography, mesoporous materials, zeolites
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-166070 (URN)978-91-7797-614-1 (ISBN)978-91-7797-615-8 (ISBN)
Public defence
2019-04-12, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (English)
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Note

At the time of the doctoral defense, the following paper was unpublished and had a status as follows: Paper 3: Manuscript.

Available from: 2019-03-20 Created: 2019-02-13 Last updated: 2020-05-15Bibliographically approved

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