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Issue 27, 2011
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Definitive solid-state 185/187Re NMR spectral evidence for and analysis of the origin of high-order quadrupole-induced effects for I = 5/2

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Abstract

Rhenium-185/187 solid-state nuclear magnetic resonance (SSNMR) experiments using NaReO4 and NH4ReO4 powders provide unambiguous evidence for the existence of high-order quadrupole-induced effects (HOQIE) in SSNMR spectra. Fine structure, not predicted by second-order perturbation theory, has been observed in the 185/187Re SSNMR spectrum of NaReO4 at 11.75 T, where the ratio of the Larmor frequency (ν0) to the quadrupole frequency (νQ) is ∼2.6. This is the first experimental observation that under static conditions, HOQIE can directly manifest in SSNMR powder patterns as additional fine structure. Using NMR simulation software which includes the quadrupole interaction (QI) exactly, extremely large 185/187Re nuclear quadrupole coupling constants (CQ) are accurately determined. QI parameters are confirmed independently using solid-state 185/187Re nuclear quadrupole resonance (NQR). We explain the spectral origin of the HOQIE and provide general guidelines that may be used to assess when HOQIE may impact the interpretation of the SSNMR powder pattern of any spin-5/2 nucleus in a large, axially symmetric electric field gradient (EFG). We also quantify the errors incurred when modeling SSNMR spectra for any spin-5/2 nucleus within an axial EFG using second-order perturbation theory. Lastly, we measure rhenium chemical shifts in the solid state for the first time.

Graphical abstract: Definitive solid-state 185/187Re NMR spectral evidence for and analysis of the origin of high-order quadrupole-induced effects for I = 5/2

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Publication details

The article was received on 01 Mar 2011, accepted on 09 May 2011 and first published on 01 Jun 2011


Article type: Paper
DOI: 10.1039/C1CP20572B
Citation: Phys. Chem. Chem. Phys., 2011,13, 12413-12420
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    Definitive solid-state 185/187Re NMR spectral evidence for and analysis of the origin of high-order quadrupole-induced effects for I = 5/2

    C. M. Widdifield, A. D. Bain and D. L. Bryce, Phys. Chem. Chem. Phys., 2011, 13, 12413
    DOI: 10.1039/C1CP20572B

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