A solid-state NMR method for solution of zeolite crystal structures

Brouwer, Darren H., Darton, Richard J., Morris, Russell E. and Levitt, Malcolm H. (2005) A solid-state NMR method for solution of zeolite crystal structures. Journal of the American Chemical Society, 127, (29), 10365-10370. (doi:10.1021/ja052306h).


PDF - Accepted Manuscript
Download (310Kb)
PDF (supporting information)
Download (840Kb)
Original Publication URL: http://dx.doi.org/10.1021/ja052306h


Since zeolites are notoriously difficult to prepare as large single crystals, structure determination usually relies on powder X-ray diffraction (XRD). However, structure solution (i.e., deriving an initial structural model) directly from powder XRD data is often very difficult due to the diffraction phase problem and the high degree of overlap between the individual reflections, particularly for materials with the structural complexity of most zeolites. Here, we report a method for structure determination of zeolite crystal structures that combines powder XRD and nuclear magnetic resonance (NMR) spectroscopy in which the crucial step of structure solution is achieved using solid-state Si-29 double-quantum dipolar recoupling NMR, which probes the distance-dependent dipolar interactions between naturally abundant Si-29 nuclei in the zeolite framework. For two purely siliceous zeolite blind test samples, we demonstrate that the NMR data can be combined with the unit cell parameters and space group to solve structural models that refine successfully against the powder XRD data.

Item Type: Article
Digital Object Identifier (DOI): doi:10.1021/ja052306h
ISSNs: 0002-7863 (print)
Related URLs:
Keywords: powder diffraction data, angle-spinning nmr, x-ray-diffraction, mas-nmr, molecular-sieves, crystallography, spectroscopy, couplings, silica, ferrierite
Subjects: Q Science > QC Physics
Q Science > QD Chemistry
T Technology > TP Chemical technology
Divisions : University Structure - Pre August 2011 > School of Chemistry
Faculty of Natural and Environmental Sciences > Chemistry > Magnetic Resonance
ePrint ID: 20741
Accepted Date and Publication Date:
27 July 2005Published
Date Deposited: 28 Feb 2006
Last Modified: 31 Mar 2016 11:38
Development of recoupling techniques in solid-state NMR
Funded by: EPSRC (GR/S40640/01)
1 October 2003 to 31 March 2007
URI: http://eprints.soton.ac.uk/id/eprint/20741

Actions (login required)

View Item View Item

Downloads from ePrints over the past year. Other digital versions may also be available to download e.g. from the publisher's website.

View more statistics