Change search
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf
Interrupted silicogermanate with 10-ring channels: synthesis and structure determination by combining rotation electron diffraction and powder X-ray diffraction
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Show others and affiliations
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.

Place, publisher, year, edition, pages
2017. Vol. 4, no 10, 1654-1659 p.
National Category
Materials Chemistry
Research subject
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-147667DOI: 10.1039/C7QI00309AISI: 000412776000007OAI: oai:DiVA.org:su-147667DiVA: diva2:1148125
Available from: 2017-10-10 Created: 2017-10-10 Last updated: 2017-11-13Bibliographically approved
In thesis
1. 3D Electron Diffraction: Application and Development towards High-quality Structure Determination
Open this publication in new window or tab >>3D Electron Diffraction: Application and Development towards High-quality Structure Determination
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
three-dimensional electron diffraction, structure determination, rotation electron diffraction
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-147732 (URN)978-91-7797-027-9 (ISBN)978-91-7797-028-6 (ISBN)
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

Open Access in DiVA

No full text

Other links

Publisher's full text

Search in DiVA

By author/editor
Wang, YunchenSu, JieWan, Wei
By organisation
Department of Materials and Environmental Chemistry (MMK)
Materials Chemistry

Search outside of DiVA

GoogleGoogle Scholar

doi
urn-nbn

Altmetric score

doi
urn-nbn
Total: 12 hits
CiteExportLink to record
Permanent link

Direct link
Cite
Citation style
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Other style
More styles
Language
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Other locale
More languages
Output format
  • html
  • text
  • asciidoc
  • rtf