Germanate with Three-Dimensional 12 x 12 x 11-Ring Channels Solved by X-ray Powder Diffraction with Charge-Flipping Algorithm
2013 (English)In: Inorganic Chemistry, ISSN 0020-1669, E-ISSN 1520-510X, Vol. 52, no 18, 10238-10244 p.Article in journal (Refereed) Published
A new open-framework germanate, denoted as GeO-JU90, was prepared by the hydrothermal synthesis method using 1,5-bis(methylpyrrolidinium)pentane dihydroxide as the organic structure-directing agent (SDA). The structure of GeO-JU90 was determined from synchrotron X-ray powder diffraction (XRPD) data using the charge-flipping algorithm. It revealed a complicated framework structure containing 11 Ge atoms in the asymmetric unit. The framework is built of 7-connected Ge-7 clusters and additional tetrahedral GeO3(OH) units forming a new three-dimensional interrupted framework with interesting 12 X 12 X 11-ring intersecting channels. The Ge K-edge extended X-ray absorption fine structure (EXAFS) analysis was performed to provide the local structural information around Ge atoms, giving rise to a first-shell contribution from about 4.2(2) O atoms at the average distance of 1.750(8) angstrom. The guest species subsequently determined by the simulated annealing method from XRPD data combining with other characterization techniques, e.g., C-13 NMR spectroscopy, infrared spectroscopy (FTIR), compositional analyses, and thermogravimetric analysis (TGA). Crystallographic data vertical bar(C15N2H32)(NH4)vertical bar[Ge11O21.5(OH)(4)], orthorhombic Ama2 (No. 40), a = 37.82959 angstrom, b = 15.24373 angstrom, c = 12.83659 angstrom, and Z = 8.
Place, publisher, year, edition, pages
2013. Vol. 52, no 18, 10238-10244 p.
IdentifiersURN: urn:nbn:se:su:diva-101026DOI: 10.1021/ic302705fISI: 000330098300008OAI: oai:DiVA.org:su-101026DiVA: diva2:699396
National Natural Science Foundation of China; State Basic Research Project of China 2011CB808703; Swedish Research Council (VR); Swedish Governmental Agency for Innovation Systems (VINNOVA) through the Berzelii Center EXSELENT; NSERC Canada; CIHR; NRC; University of Saskatchewan 2014-02-272014-02-212014-04-23Bibliographically approved