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Open-Framework Germanates: Crystallography, structures and cluster building units
Stockholm University, Faculty of Science, Department of Physical, Inorganic and Structural Chemistry.
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis is focussing on the crystallographic challenges and what knowledge we can gain from studying the different open-framework germanates. Five new open-framework germanates have been synthesized and the structures have been determined by single crystal X-ray diffraction. A thorough description is made of the different problems raised with the different compounds, whether it is choice of crystal system in SU-61, twinning and possible ordering in SU-46, superstructure and variation in elemental content in SU-57, template disorder in JLG-5 or framework disorder in SU-44.

Open-framework germanates are often built from one type of cluster, such as the Ge7 [Ge7X19], Ge8 [Ge8X20], Ge9 [Ge9Xn, n =25-26] and Ge10 [Ge10X28], (X =O, OH, F) clusters. The structures built by clusters containing different kinds of polyhedra are discussed, with a focus on the 4-coordinated Ge7 clusters, the larger cluster aggregate found in SU-8 and SU-44 and the structures built by the Ge10 clusters.

Place, publisher, year, edition, pages
Stockholm: Institutionen för fysikalisk kemi, oorganisk kemi och strukturkemi , 2008. , 90 p.
Keyword [en]
germanate, crystallography, building unit, zeotype, scale chemistry
National Category
Chemical Sciences
Research subject
Structural Chemistry
Identifiers
URN: urn:nbn:se:su:diva-7501ISBN: 978-91-7155-570-0 (print)OAI: oai:DiVA.org:su-7501DiVA: diva2:198435
Public defence
2008-05-16, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 12 A, Stockholm, 10:00
Opponent
Supervisors
Available from: 2008-04-24 Created: 2008-04-24Bibliographically approved
List of papers
1. An open-framework silicogermanate with 26-ring channels built from seven-coordinated (Ge,Si)10(O, OH)28 clusters
Open this publication in new window or tab >>An open-framework silicogermanate with 26-ring channels built from seven-coordinated (Ge,Si)10(O, OH)28 clusters
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2008 (English)In: Journal of the American Chemical Society, ISSN 0002-7863, E-ISSN 1520-5126, Vol. 130, no 12, 3758-3759 p.Article in journal (Refereed) Published
Abstract [en]

We report a new open-framework silicogermanate SU-61 containing 26-ring channels with a low framework density. It can be seen as a crystalline analogue to the mesoporous silica MCM-41. The structure is built from the assembly of (Ge,Si)10(O,OH)28 clusters. It is the first time that silicon has been successfully introduced in the Ge10 cluster in significant amounts (21% of the tetrahedral sites). Five- and six-coordinated Ge10 clusters have previously been observed in other germanate compounds leading to either dense or open structures. In SU-61, the seven-coordinated clusters fall onto yet another underlying net, the osf net. SU-61, along with other Ge10 based frameworks, shows the versatility of the germanate system to adopt defined topologies playing on the connectivity of the clusters following the principles of net decoration and scale chemistry.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:su:diva-24856 (URN)10.1021/ja8002556 (DOI)000254173600027 ()
Available from: 2008-04-24 Created: 2008-04-24 Last updated: 2012-03-08Bibliographically approved
2. Synthesis and characterization of an aluminogermanate SU-46 with a zeolite structure
Open this publication in new window or tab >>Synthesis and characterization of an aluminogermanate SU-46 with a zeolite structure
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2007 In: Chemistry of Materials, ISSN 0897-4756, Vol. 19, no 24, 5973-5979 p.Article in journal (Refereed) Published
Identifiers
urn:nbn:se:su:diva-24857 (URN)000251150900031 ()
Note
Part of urn:nbn:se:su:diva-7501Available from: 2008-04-24 Created: 2008-04-24Bibliographically approved
3. SU-57 – An aluminosilicogermanate with a DFT topology and variable compositions
Open this publication in new window or tab >>SU-57 – An aluminosilicogermanate with a DFT topology and variable compositions
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2009 (English)In: Microporous and Mesoporous Materials, ISSN 1387-1811, Vol. 117, no 1-2, 285-291 p.Article in journal (Refereed) Published
Abstract [en]

An aluminosilicogermanate with a DFT zeotype framework (denoted as SU-57) was synthesized for the first time by ethanol-assisted hydrothermal synthesis at 160 and 170 °C. The compound was characterized by single crystal and powder X-ray diffraction, scanning and transmission electron microscopy, energy dispersive spectroscopy (EDS), thermogravimetry (TG) and solid state nuclear magnetic resonance (NMR) spectroscopy. SU-57 crystallizes in space group P42/n with estimated a ≈ 10.38–10.46 Å, c ≈ 8.88–8.91 Å, V ≈ 957–975 Å3. It has variable Al–Si–Ge composition with an approximate formula |C2H10N2| [Al(SixGe1−x)O4]2 (x ≈ 0.3–0.9), which results in a super-structure originated from different cation occupancies of the two unique tetrahedral (T) sites. Single crystal X-ray structure refinements, together with results from X-ray powder diffraction (XRPD) and EDS analysis, showed that (i) the AlO4 and (Si, Ge)O4 tetrahedra are only partially ordered over the DFT framework and do not follow a strict alternating manner. (ii) Al resides predominantly on one T site and Si and Ge predominantly on the other. (iii) The Al cation concentration (Al/(Al + Si + Ge)) is nearly constant and slightly less than 50 at%, while the Si and Ge cation concentrations vary over a large range. (iv) Al and Ge occupy both T sites. The cation disorder was confirmed by 27Al and 29Si solid state NMR. TG analysis and in situ XRPD showed that SU-57 was stable up to 375 °C in N2 atmosphere.

Keyword
Aluminosilicogermanate, DFT zeotype, Hydrothermal synthesis, X-ray diffraction, Energy dispersive spectroscopy, 27Al and 29Si solid state NMR
National Category
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-24858 (URN)10.1016/j.micromeso.2008.06.036 (DOI)000262879700037 ()
Available from: 2008-04-24 Created: 2008-04-24 Last updated: 2011-09-20Bibliographically approved
4. A germanate built from from 68126 cavity co-templated by a (H2O)16 water cluster and 2-methylpiperazine
Open this publication in new window or tab >>A germanate built from from 68126 cavity co-templated by a (H2O)16 water cluster and 2-methylpiperazine
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2008 (English)In: Angewandte Chemie International Edition, ISSN 1433-7851, E-ISSN 1521-3773Article in journal (Refereed) Submitted
National Category
Organic Chemistry
Identifiers
urn:nbn:se:su:diva-24859 (URN)
Note

Part of urn:nbn:se:su:diva-7501

Available from: 2008-04-24 Created: 2008-04-24 Last updated: 2015-10-16Bibliographically approved
5. Design of Open-Framework Germanates by Combining Different Building Units
Open this publication in new window or tab >>Design of Open-Framework Germanates by Combining Different Building Units
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2006 In: Journal of American Chemical Society, ISSN 0002-7863, Vol. 128, no 44, 14238-14239 p.Article in journal (Refereed) Published
Identifiers
urn:nbn:se:su:diva-24860 (URN)
Note
Part of urn:nbn:se:su:diva-7501Available from: 2008-04-24 Created: 2008-04-24Bibliographically approved
6. Open-framework germanates formed by the flexible Ge10 cluster
Open this publication in new window or tab >>Open-framework germanates formed by the flexible Ge10 cluster
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2008 (English)In: Zeolites and related materials: Trends, targets and challenges: Proceedings of the 4th International FEZA Conference, Vol. 174, Part A / [ed] Antoine Gédéon, Pascale Massiani and Florence Babonneau, Amsterdam: Elsevier, 2008, 317-320 p.Conference paper, Published paper (Refereed)
Abstract [en]

Open-framework germanates have shown promising results in achieving extra-large pores and channels. Pores that extend to the mesoporous range (>20Å) were reported in SU-M. The structure of SU-M is built by the Ge10X28 (Ge10, X = O, OH, F) clusters. This cluster is also found in Ge-pharmacosiderite, Na4Ge9O20, ICMM-7 and SU-61. The Ge10 cluster has a flexibility to form compounds with both high and very low framework densities.

Place, publisher, year, edition, pages
Amsterdam: Elsevier, 2008
Series
Studies in surface science and catalysis, ISSN 0167-2991
Keyword
Open-framework germanate, Ge10 cluster, coordination, crystal structure
National Category
Chemical Sciences
Identifiers
urn:nbn:se:su:diva-24861 (URN)10.1016/S0167-2991(08)80206-6 (DOI)978-0-444-53297-8 (ISBN)
Conference
Paris, France, 2-6 September 2008
Available from: 2008-04-24 Created: 2008-04-24 Last updated: 2012-03-08Bibliographically approved
7. Design of three-dimensional open-framework structures from inorganic clusters
Open this publication in new window or tab >>Design of three-dimensional open-framework structures from inorganic clusters
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2007 In: From Zeolites to Porous MOF Materials - the 40th Anniversary of International Zeolite Conference, 170: Proceedings of the 15th International Zeolite Conference, Beijing, P. R. China, 12-17th August 2007, Elsevier , 2007, 682-689 p.Chapter in book (Other academic) Published
Place, publisher, year, edition, pages
Elsevier, 2007
Identifiers
urn:nbn:se:su:diva-24862 (URN)978-0-444-53068-4 (ISBN)
Note
Part of urn:nbn:se:su:diva-7501Available from: 2008-04-24 Created: 2008-04-24Bibliographically approved

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