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  • Title: Measurement of 13C-1H dipolar couplings in solids by using ultra-fast magic-angle spinning NMR spectroscopy with symmetry-based sequences.
    Author: Wang Q, Lu X, Lafon O, Trébosc J, Deng F, Hu B, Chen Q, Amoureux JP.
    Journal: Phys Chem Chem Phys; 2011 Apr 07; 13(13):5967-73. PubMed ID: 21336406.
    Abstract:
    We show that (13)C-(1)H 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 (13)C-(1)H dipolar couplings are recovered by using the R12 recoupling scheme, while the interference of (1)H-(1)H dipolar couplings are suppressed by the symmetry properties of this sequence and the use of high MAS frequency (65 kHz). The R12 method is especially advantageous for large (13)C-(1)H 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 (13)C-(1)H 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.
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