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Investigation of the effect of polar functional groups on the crystal structures of indium MOFs
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Number of Authors: 4
2017 (English)In: CrystEngComm, ISSN 1466-8033, E-ISSN 1466-8033, Vol. 19, no 31, 4622-4628 p.Article in journal (Refereed) Published
Abstract [en]

Three new In-MOFs with -NH2 and/or -NO2 functionalities are reported using 2-amino-(H2BDC-NH2), 2-nitro-(H2BDC-NO2) and 2-amino-5-nitroterephthalic acid (H2BDC-NH2/NO2). Their structures were determined from single crystal X-ray diffraction data. The structure of the first In-MOF of composition [In(BDC-NH3)(BDC-NH2)] center dot 1.6DMF center dot 1.9H(2)O (In-BDC-NH2;DMF is dimethylformamide; the space group is P6(2)22, a = b = 14.738(2) angstrom and c = 12.257(3) angstrom) is built up by two interpenetrating nets of InOB polyhedra interconnected by BDC-NH2 2-ions to form a framework with qtz topology. Charge balance is accomplished by partial protonation of the amino group, which was confirmed by IR spectroscopy. The interpenetration leads to a decrease of the pore dimension (4.4 angstrom in diameter). Thermogravimetric analysis revealed stability up to 300 degrees C. Replacement of H2BDC-NH2 by H2BDC-NO2 in the reaction mixture led to the iso-reticular MOF containing no -NO2 groups but exclusively un- and amino-functionalized linkers. Hence an indium mediated reduction of the H2BDC-NO2 linker molecule during solvothermal synthesis has occurred. The use of H2BDC-NH2/NO2 under exactly the same reaction conditions did not result in the formation of a MOF, but by changing the synthesis parameters, a new -NH2/-NO2 bifunctionalised In-MOF of composition (DMA)(2).In-3.mu(3)-O)(BDC-NH2/NO2) 4.5] center dot DMF (DMA is dimethylammonium), denoted In-BDC-NH2/NO2, was obtained. The crystal morphology can be altered from cubic to truncated octahedral crystals by varying the DMF/ethanol volume ratio during synthesis. The compound crystallises in the cubic space group I43m, a = 24.8947(1) angstrom, and the framework contains trinuclear {In-3.mu(3)-O)} clusters which are interlinked by the BDC-NH2/NO2 2-ions to form super-tetrahedra. Four face-sharing super-tetrahedra form ultra-tetrahedra which are connected to form the final cubic framework with an ncb topology and isolated inaccessible pores.

Place, publisher, year, edition, pages
2017. Vol. 19, no 31, 4622-4628 p.
National Category
Chemical Sciences
Identifiers
URN: urn:nbn:se:su:diva-147069DOI: 10.1039/c7ce01067bISI: 000407300500021OAI: oai:DiVA.org:su-147069DiVA: diva2:1142327
Available from: 2017-09-19 Created: 2017-09-19 Last updated: 2017-09-19Bibliographically approved

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