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3D Electron Diffraction: Application and Development towards High-quality Structure Determination
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
2017 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Electron crystallography has been proven to be effective for structure determination of nano- and micron-sized crystals. In the past few years, 3D electron diffraction (3DED) techniques were used for the structure solution of various types of complex structures such as zeolites, metal-organic frameworks (MOF) and pharmaceutical compounds. However, unlike X-ray crystallography, electron diffraction has not yet become an independent technique for a complete structure determination due to relatively poorer diffraction intensities and often powder X-ray diffraction data are used for structure validation and refinement.

Electron beam damage to the structures that are sensitive to high energy electrons and dynamical scattering are important factors to lead to the deviation of electron diffraction intensities from the squared amplitudes of the structure factors. In this thesis, we investigate various aspects around the 3D electron diffraction data quality and strategies for obtaining better data and structure models. We combined 3D electron diffraction methods and powder X-ray diffraction to determine the structure of an open-framework material and discussed the difficulties and limitations of electron diffraction for beam sensitive materials. Next, we illustrated the structure determination of a pharmaceutical compound, bismuth subgallate, using 3D electron diffraction. While severe beam damage and diffuse scattering were observed in the dataset collected with the conventional rotation electron diffraction (RED) method, the continuous rotation electron diffraction (cRED) method coupled with sample cooling significantly improved the data quality and made the structure solution possible. In order to better understand the potentials and limitations of the continuous rotation method, we collected multiple datasets from different crystals of a known structure and studied the data quality by evaluating the accuracy of the refined structure models. To tackle dynamical scattering in electron diffraction data, we explored a routine for structure refinement with dynamical intensity calculation using RED data from a known structure and discussed its potentials and limitations.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry, Stockholm University , 2017. , 73 p.
Keyword [en]
three-dimensional electron diffraction, structure determination, rotation electron diffraction
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-147732ISBN: 978-91-7797-027-9 (print)ISBN: 978-91-7797-028-6 (electronic)OAI: oai:DiVA.org:su-147732DiVA: diva2:1148356
Public defence
2017-11-24, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Note

At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 3: Manuscript. Paper 4: Manuscript.

Available from: 2017-10-31 Created: 2017-10-10 Last updated: 2017-11-01Bibliographically approved
List of papers
1. Interrupted silicogermanate with 10-ring channels: synthesis and structure determination by combining rotation electron diffraction and powder X-ray diffraction
Open this publication in new window or tab >>Interrupted silicogermanate with 10-ring channels: synthesis and structure determination by combining rotation electron diffraction and powder X-ray diffraction
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2017 (English)In: Inorganic Chemistry Frontiers, ISSN 2052-1553, Vol. 4, no 10, 1654-1659 p.Article in journal (Refereed) Published
Abstract [en]

Silicogermanate (JU110) with an interrupted open-framework has been synthesized by using a hydrothermal method using 1,1′-(1,4-phenylenebis(methylene))bis(1-methylpyrrolidin-1-ium) hydroxide as an organic structure-directing agent (OSDA). Silicon and fluoride anions were introduced to the concentrated-gel synthesis system, and different synthetic parameters influencing the synthesis were discussed. The structure of JU110 was characterised by using rotation electron diffraction (RED) and high-resolution powder X-ray diffraction. JU110 crystallizes in the space group Fm2m (No. 42) with a = 13.9117(2) Å, b = 18.2980(3) Å and c = 32.7800(6) Å. The structure is constructed by the sti layers found in the STI framework that are pillared by D4R/Ge7 units to form a large cavity, showing 10-ring openings along [100] and 9-ring openings along [110]. Thermal stability studies showed that the framework was maintained with the loss of water molecules, but collapsed with the removal of charge-compensating cations.

National Category
Materials Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-147667 (URN)10.1039/C7QI00309A (DOI)000412776000007 ()
Available from: 2017-10-10 Created: 2017-10-10 Last updated: 2017-11-13Bibliographically approved
2. Elucidation of the elusive structure and formula of the active pharmaceutical ingredient bismuth subgallate by continuous rotation electron diffraction
Open this publication in new window or tab >>Elucidation of the elusive structure and formula of the active pharmaceutical ingredient bismuth subgallate by continuous rotation electron diffraction
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2017 (English)In: Chemical Communications, ISSN 1359-7345, E-ISSN 1364-548X, Vol. 53, no 52, 7018-7021 p.Article in journal (Refereed) Published
Abstract [en]

Bismuth subgallate has been used in wound and gastrointestinal therapy for over a century. The combination of continuous rotation electron diffraction and sample cooling finally revealed its structure as a coordination polymer. The structure provides insight regarding its formula, poor solubility, acid resistance and previously unreported gas sorption properties.

National Category
Materials Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-145991 (URN)10.1039/c7cc03180g (DOI)000404466200008 ()28613325 (PubMedID)
Available from: 2017-08-29 Created: 2017-08-29 Last updated: 2017-10-10Bibliographically approved
3. On the quality of the continuous rotation electron diffraction data for accurate atomic structure determination of inorganic compounds
Open this publication in new window or tab >>On the quality of the continuous rotation electron diffraction data for accurate atomic structure determination of inorganic compounds
(English)Manuscript (preprint) (Other academic)
National Category
Materials Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-147656 (URN)
Available from: 2017-10-09 Created: 2017-10-09 Last updated: 2017-11-03Bibliographically approved
4. Dynamical structure refinement of Ni3Si2 against rotation electron diffraction data
Open this publication in new window or tab >>Dynamical structure refinement of Ni3Si2 against rotation electron diffraction data
(English)Manuscript (preprint) (Other academic)
National Category
Materials Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-147658 (URN)
Available from: 2017-10-09 Created: 2017-10-09 Last updated: 2017-11-03Bibliographically approved

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