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Central-transition double-quantum sideband NMR spectroscopy of half-integer quadrupolar nuclei: estimating internuclear distances and probing clusters within multi-spin networks
Stockholms universitet, Naturvetenskapliga fakulteten, Institutionen för material- och miljökemi (MMK).
2014 (engelsk)Inngår i: Physical Chemistry, Chemical Physics - PCCP, ISSN 1463-9076, E-ISSN 1463-9084, Vol. 16, nr 15, s. 7037-7050Artikkel i tidsskrift (Fagfellevurdert) Published
Abstract [en]

We introduce a strategy to estimate the size of clusters of recoupled homonuclear half-integer quadrupolar nuclei under magic-angle spinning (MAS) conditions, by combining double-quantum (2Q) sideband NMR experiments with an approximate numerical analysis based on the summation of all spin-pairs present over a given radius of the structure. The experiment relies solely on the evolution of homonuclear 2Q coherences (2QC) among the central-transitions (CT) of half-integer spins and is suitable for probing clusters in network structures, such as those encountered in large groups of oxide-based materials. Experimental B-11, Na-23 and Al-27 NMR results are presented on bis(catecholato)diboron, Na2SO4 and Al2O3, respectively; in each case, the growth of the spin-cluster size was monitored from a series of experiments that employed progressively lengthened 2QC excitation intervals. Our new approach is the first option for probing larger constellations of half-integer spins; it provides similar information as the multiple-quantum spin counting experiment, which is well-established for spin-1/2 applications but has hitherto not been demonstrated for half-integer spins undergoing MAS. We also discuss various options for determining the internuclear distance within a (nearly) isolated pair of half-integer spins by comparing the experimental 2Q sideband NMR spectra with results from numerical simulations involving various degrees of approximation.

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2014. Vol. 16, nr 15, s. 7037-7050
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URN: urn:nbn:se:su:diva-102802DOI: 10.1039/c4cp00029cISI: 000333121300027OAI: oai:DiVA.org:su-102802DiVA, id: diva2:713371
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AuthorCount:2;

Tilgjengelig fra: 2014-04-22 Laget: 2014-04-22 Sist oppdatert: 2017-12-05bibliografisk kontrollert

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