Central-transition double-quantum sideband NMR spectroscopy of half-integer quadrupolar nuclei: Estimating internuclear distances and probing clusters within multi-spin networks

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DOIResolve DOI: http://doi.org/10.1039/c4cp00029c
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TypeArticle
Journal titlePhysical Chemistry Chemical Physics
ISSN1463-9076
Volume16
Issue15
Pages70377050; # of pages: 14
AbstractWe 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 11B, 23Na and 27Al NMR results are presented on bis(catecholato)diboron, Na2SO4 and Al 2O3, 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. © 2014 the Partner Organisations.
Publication date
LanguageEnglish
AffiliationNational Research Council Canada (NRC-CNRC); Measurement Science and Standards (MSS-SME)
Peer reviewedYes
NPARC number21272181
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Record identifierb8201b08-2b23-4b58-b210-b5c9c3698f94
Record created2014-07-23
Record modified2016-05-09
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