Issue 27, 2014

Ab initio structure determination of interlayer expanded zeolites by single crystal rotation electron diffraction

Abstract

Layered solids often form thin plate-like crystals that are too small to be studied by single-crystal X-ray diffraction. Although powder X-ray diffraction (PXRD) is the conventional method for studying such solids, it has limitations because of peak broadening and peak overlapping. We have recently developed a software-based rotation electron diffraction (RED) method for automated collection and processing of 3D electron diffraction data. Here we demonstrate the ab initio structure determination of two interlayer expanded zeolites, the microporous silicates COE-3 and COE-4 (COE-n stands for International Network of Centers of Excellence-n), from submicron-sized crystals by the RED method. COE-3 and COE-4 are built of ferrierite-type layers pillared by (–O–Si(CH3)2–O–) and (–O–Si(OH)2–O–) linker groups, respectively. The structures contain 2D intersecting 10-ring channels running parallel to the ferrierite layers. Because both COE-3 and COE-4 are electron-beam sensitive, a combination of RED datasets from 2 to 3 different crystals was needed for the structure solution and subsequent structure refinement. The structures were further refined by Rietveld refinement against the PXRD data. The structure models obtained from RED and PXRD were compared.

Graphical abstract: Ab initio structure determination of interlayer expanded zeolites by single crystal rotation electron diffraction

Supplementary files

Article information

Article type
Paper
Submitted
13 feb 2014
Accepted
14 apr 2014
First published
15 apr 2014

Dalton Trans., 2014,43, 10593-10601

Author version available

Ab initio structure determination of interlayer expanded zeolites by single crystal rotation electron diffraction

P. Guo, L. Liu, Y. Yun, J. Su, W. Wan, H. Gies, H. Zhang, F. Xiao and X. Zou, Dalton Trans., 2014, 43, 10593 DOI: 10.1039/C4DT00458B

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