A solid-state NMR method for solution of zeolite crystal structures
A solid-state NMR method for solution of zeolite crystal structures
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.
powder diffraction data, angle-spinning nmr, x-ray-diffraction, mas-nmr, molecular-sieves, crystallography, spectroscopy, couplings, silica, ferrierite
10365-10370
Brouwer, Darren H.
e9ad5763-0b22-4734-831f-22ead41ada1d
Darton, Richard J.
d6c37816-dfbf-492f-9826-786e1441165d
Morris, Russell E.
c882b263-3800-45b4-b342-04684c68adf8
Levitt, Malcolm H.
bcc5a80a-e5c5-4e0e-9a9a-249d036747c3
27 July 2005
Brouwer, Darren H.
e9ad5763-0b22-4734-831f-22ead41ada1d
Darton, Richard J.
d6c37816-dfbf-492f-9826-786e1441165d
Morris, Russell E.
c882b263-3800-45b4-b342-04684c68adf8
Levitt, Malcolm H.
bcc5a80a-e5c5-4e0e-9a9a-249d036747c3
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), .
(doi:10.1021/ja052306h).
Abstract
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.
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DB_zeolites2_reprint.pdf
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DB_zeolites2_SI.pdf
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More information
Published date: 27 July 2005
Keywords:
powder diffraction data, angle-spinning nmr, x-ray-diffraction, mas-nmr, molecular-sieves, crystallography, spectroscopy, couplings, silica, ferrierite
Organisations:
Magnetic Resonance
Identifiers
Local EPrints ID: 20741
URI: http://eprints.soton.ac.uk/id/eprint/20741
ISSN: 0002-7863
PURE UUID: 3a89b7bc-6775-4cb4-813c-adef345d32ca
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Date deposited: 28 Feb 2006
Last modified: 16 Mar 2024 03:18
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Contributors
Author:
Darren H. Brouwer
Author:
Richard J. Darton
Author:
Russell E. Morris
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