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Layered V-B-O Polyoxometalate Nets Linked by Diethylenetriamine Complexes with Dangling Amine Groups
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). China University of Geosciences - Wuhan, People's Republic of China.
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Peking University, People's Republic of China.
2014 (English)In: Dalton Transactions, ISSN 1477-9226, E-ISSN 1477-9234, Vol. 43, no 41, 15283-15286 p.Article in journal (Refereed) Published
Abstract [en]

Two layered V-B-O contained polyoxometalate (POM) net structures, denoted as SUT-12 and SUT-13, are reported here. SUT-12 was synthesized by the boric acid flux method, and it represents the first 2D structure constructed from the V6B20 vanadoborate cluster. SUT-13 was synthesized through the hydrothermal method and constructed from V12B6P12 vanadium borophosphate clusters. In both structures, the vanadoborate or vanadium borophosphate clusters were linked through in-situ formed Zn(DETA)2 or Cu(DETA)2 complexes. Surprisingly, for all DETA molecules in the two metal complexes, there is one dangling amine group when it coordinated to the metal. The phenomena of the dangling amine group feature is abnormal and the Cu(DETA)2 complexes in SUT-13 was taken as an example and studied by density function theory (DFT) calculation in order to understand this unusual feature.

Place, publisher, year, edition, pages
2014. Vol. 43, no 41, 15283-15286 p.
National Category
Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-106861DOI: 10.1039/C4DT01533AISI: 000342757600003OAI: oai:DiVA.org:su-106861DiVA: diva2:740563
Available from: 2014-08-25 Created: 2014-08-25 Last updated: 2017-12-05Bibliographically approved
In thesis
1. Open-framework Structures Built by Inorganic Clusters: Synthesis and Characterization
Open this publication in new window or tab >>Open-framework Structures Built by Inorganic Clusters: Synthesis and Characterization
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Novel open-framework germanates and vanadoborates, which are constructed from typical types of clusters, have been synthesized based on different strategies. The crystal structures are solved by using single crystal X-ray diffraction (SXRD) technique or by combined techniques. Additionally, the structures of two open-framework materials, PKU-3 and PKU-16, are determined from nano-sized crystals by rotation electron diffraction (RED) combined with powder X-ray diffraction (PXRD).

This thesis serves as an introduction to synthesis of open-framework germanates and vanadoborates based on different design strategies. Two germanates are obtained; SU-74 is achieved by employing a novel structure directing agent (SDA), SUT-8 is achieved by assembling the novel structure building units (SBUs) of Co@Ge14 with the introduction of cobalt ions in the synthesis. Four strategies are successfully used in construction of open-framework vanadoborates: using metal-oxo polyhedra as the linkages in SUT-6; applying the scale chemistry approach in SUT-7; employing metal-organic complexes as the linkages in SUT-12, SUT-13, SUT-14; and introducing covalent bond organic linkages into SUT-10 and SUT-11. Single crystal X-ray diffraction is used to conduct the structure determination in combination with other techniques.

Furthermore, the structures of two open-framework materials, an aluminoborate PKU-3 and a germanosilicate PKU-16, are solved from nano-sized crystals using RED data. The structures are further confirmed by Rietveld refinement against PXRD data. The advantages of the RED techniques are demonstrated in two aspects. In PKU-3, the presence of seriously preferred orientation and light elements in the structure makes it difficult for structure determination by PXRD, but it is easier by RED. In PKU-16, the RED technique is used to determine its structure from the as-synthesized multi-phasic sample containing nano-sized crystals. After the structure of PKU-16 has been solved, the synthesis of this interesting phase can be optimized and pure PKU-16 can be obtained.

Keywords: Open-framework, germanates, vanadoborates, aluminoborates, germanosilicates, crystal structure, hydrothermal synthesis, single crystal X-ray diffraction, rotation electron diffraction, powder X-ray diffraction

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm Univeristy, 2014. 87 p.
Keyword
Open-framework, germanates, vanadoborates, aluminoborates, germanosilicates, crystal structure, hydrothermal synthesis, crystal X-ray diffraction, rotation electron diffraction, powder X-ray diffraction
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-106853 (URN)978-91-7447-962-1 (ISBN)
Public defence
2014-09-29, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (English)
Opponent
Supervisors
Available from: 2014-09-07 Created: 2014-08-25 Last updated: 2014-09-15Bibliographically approved

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