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Issue 13, 2011
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Measurement of 13C–1H dipolar couplings in solids by using ultra-fast magic-angle spinning NMR spectroscopy with symmetry-based sequences

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Abstract

We show that 13C–1H dipolar couplings in fully protonated organic solids can be measured by applying a Symmetry-based Resonance-Echo DOuble-Resonance (S-REDOR) experiment at ultra-fast Magic-Angle Spinning (MAS). The 13C–1H dipolar couplings are recovered by using the R1253 recoupling scheme, while the interference of 1H–1H dipolar couplings are suppressed by the symmetry properties of this sequence and the use of high MAS frequency (65 kHz). The R1253 method is especially advantageous for large 13C–1H dipolar interactions, since the dipolar recoupling time can be incremented by steps as short as one rotor period. This allows a fine sampling for the rising part of the dipolar dephasing curve. We demonstrate experimentally that one-bond 13C–1H dipolar coupling in the order of 22 kHz can be accurately determined. Furthermore, the proposed method allows a rapid evaluation of the dipolar coupling by fitting the S-REDOR dipolar dephasing curve with an analytical expression.

Graphical abstract: Measurement of 13C–1H dipolar couplings in solids by using ultra-fast magic-angle spinning NMR spectroscopy with symmetry-based sequences

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Publication details

The article was received on 22 Sep 2010, accepted on 19 Jan 2011 and first published on 21 Feb 2011


Article type: Paper
DOI: 10.1039/C0CP01907K
Citation: Phys. Chem. Chem. Phys., 2011,13, 5967-5973
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    Measurement of 13C–1H dipolar couplings in solids by using ultra-fast magic-angle spinning NMR spectroscopy with symmetry-based sequences

    Q. Wang, X. Lu, O. Lafon, J. Trébosc, F. Deng, B. Hu, Q. Chen and J. Amoureux, Phys. Chem. Chem. Phys., 2011, 13, 5967
    DOI: 10.1039/C0CP01907K

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