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SU-62: Synthesis and Structure Investigation of a Germanate with a Novel Three-Dimensional Net and Interconnected 10- and 14-Ring Channels
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).
2012 (English)In: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 12, no 1, 369-375 p.Article in journal (Refereed) Published
Abstract [en]

A novel 3D open-framework germanate, vertical bar N(2)C(4)H(14)vertical bar(4) [Ge(20)O(41)(OH)(6)]center dot 3H(2)O (SU-62), was prepared from hydrothermal synthesis using 1,4-diaminobutane as the organic structure directing agent (SDA). The crystal structure was solved by single crystal X-ray diffraction. The framework is built from Ge(10)(O,OH)(27) (Ge(10)) secondary building units and exhibits an irregular three-dimensional channel system encircled by 10- and 14-rings. The framework of SU-62 has an underlying topology that follows a novel five-coordinated svh-5-I4(1)/amd net, while the pores follow the tsi net. The thermal behavior of SU-62 was studied by thermogravimetric (TG) analysis and in situ X-ray diffraction (XRPD). Crystallographic data: orthorhombic, space group Fdd2, unit cell parameters a = 15.297(3) angstrom, b = 53.58(1) angstrom, c = 14.422(3) angstrom, V = 11821(4) angstrom(3), Z = 8.

Place, publisher, year, edition, pages
2012. Vol. 12, no 1, 369-375 p.
National Category
Inorganic Chemistry
Research subject
Structural Chemistry
Identifiers
URN: urn:nbn:se:su:diva-75668DOI: 10.1021/cg201482nISI: 000298726300050OAI: oai:DiVA.org:su-75668DiVA: diva2:518443
Available from: 2012-05-04 Created: 2012-04-24 Last updated: 2017-12-07Bibliographically approved
In thesis
1. Open-Framework Germanates: Synthesis, Structure, and Characterization
Open this publication in new window or tab >>Open-Framework Germanates: Synthesis, Structure, and Characterization
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Novel open-framework germanates and open low-dimensional structures were synthesized and characterized. Their crystal structures were solved by single crystal X-ray diffraction or X-ray powder diffraction combined with other techniques. Although related open-framework materials, such as zeolites, are of interest for the ability to selectively accommodate guest species in their rings, pores and channels, germanates are primarily of interest for their unique structural properties. Compared to aluminosilicate-based zeolites, germanium oxides readily form frameworks with extra-large rings and low framework density. The formation of elegant germanate architectures is attributed to the unique Ge-O bond geometries compared to Si-O, and the tendency to form large clusters.

This thesis is to serve as an introduction to germanate synthesis, structures and characterization. Structures are categorized in accordance to their building units; the Ge7X19 (Ge7), Ge9X25-26 (Ge9) and Ge10X28 (Ge10) (X = O, OH, or F) clusters. Structure determination techniques as well as the characterization techniques used to examine the properties of the materials are presented. While most of the discussed techniques have routinely been used to study crystalline open-frameworks, we introduce the use of infrared spectroscopy for the identification of cluster types, valuable for structure determination by X-ray powder diffraction. Structures and properties of the novel materials ASU-21, SU-62, SU-63, SU-64, SU-65, SU-66, SU-71, SU-72, SU-73, SU-74, SU-75 and SU-JU-14 are described and put into context with previously known structures. The novel structures are all built of the Ge7, Ge9 or Ge10 clusters, and vary from a framework with novel topology to the first open zero-dimensional germanate cavities built of such clusters.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2012. 120 p.
Keyword
Open-framework, zeolites, germanates, porous materials, crystallography, hydrothermal synthesis, crystal structure
National Category
Inorganic Chemistry
Research subject
Structural Chemistry
Identifiers
urn:nbn:se:su:diva-75732 (URN)978-91-7447-519-7 (ISBN)
Public defence
2012-06-13, 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 2: Submitted. Paper 3: Manuscript. Paper 4: Submitted. Paper 6: Submitted. Paper 7: Manuscript. Paper 8. Manuscript. Paper 10: Unpublished book chapter.

 

Available from: 2012-05-10 Created: 2012-04-26 Last updated: 2012-10-25Bibliographically approved

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