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Germanate with Three-Dimensional 12 × 12 × 11-Ring Channels Solved by X-ray Powder Diffraction with Charge-Flipping Algorithm

DOI: 10.1021/ic302705f DOI Help

Authors: Yan Xu (Jilin University) , Leifeng Liu (Stockholm University) , Daniel M. Chevrier (Dalhousie University) , Junliang Sun (Stockholm University) , Peng Zhang (Dalhousie University) , Jihong Yu (Jilin University)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Inorganic Chemistry , VOL 52 (18)

State: Published (Approved)
Published: February 2013

Abstract: 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 Ge7 clusters and additional tetrahedral GeO3(OH) units forming a new three-dimensional interrupted framework with interesting 12 × 12 × 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) Å. The guest species in the channels were subsequently determined by the simulated annealing method from XRPD data combining with other characterization techniques, e.g., 13C NMR spectroscopy, infrared spectroscopy (FTIR), compositional analyses, and thermogravimetric analysis (TGA). Crystallographic data |(C15N2H32)(NH4)|[Ge11O21.5(OH)4], orthorhombic Ama2 (No. 40), a = 37.82959 Å, b = 15.24373 Å, c = 12.83659 Å, and Z = 8.

Subject Areas: Chemistry

Instruments: I11-High Resolution Powder Diffraction

Added On: 19/02/2013 12:38

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