Rapid Natural-Abundance 2D 13C–13C Correlation Spectroscopy Using Dynamic Nuclear Polarization Enhanced Solid-State NMR and Matrix-Free Sample Preparation

Authors

  • Dr. Hiroki Takahashi,

    1. Laboratoire de Chimie Inorganique et Biologique, UMR-E3 CEA/UJF & CNRS, Institut Nanosciences et Cryogénie (CEA/DSM), 38054 Grenoble (France)
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  • Dr. Daniel Lee,

    1. Laboratoire de Chimie Inorganique et Biologique, UMR-E3 CEA/UJF & CNRS, Institut Nanosciences et Cryogénie (CEA/DSM), 38054 Grenoble (France)
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  • Dr. Lionel Dubois,

    1. Laboratoire de Chimie Inorganique et Biologique, UMR-E3 CEA/UJF & CNRS, Institut Nanosciences et Cryogénie (CEA/DSM), 38054 Grenoble (France)
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  • Dr. Michel Bardet,

    1. Laboratoire de Chimie Inorganique et Biologique, UMR-E3 CEA/UJF & CNRS, Institut Nanosciences et Cryogénie (CEA/DSM), 38054 Grenoble (France)
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  • Dr. Sabine Hediger,

    1. Laboratoire de Chimie Inorganique et Biologique, UMR-E3 CEA/UJF & CNRS, Institut Nanosciences et Cryogénie (CEA/DSM), 38054 Grenoble (France)
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  • Dr. Gaël De Paëpe

    Corresponding author
    1. Laboratoire de Chimie Inorganique et Biologique, UMR-E3 CEA/UJF & CNRS, Institut Nanosciences et Cryogénie (CEA/DSM), 38054 Grenoble (France)
    • Laboratoire de Chimie Inorganique et Biologique, UMR-E3 CEA/UJF & CNRS, Institut Nanosciences et Cryogénie (CEA/DSM), 38054 Grenoble (France)
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  • This work was supported by the ANR (ANR08-CEXC-003-01 and ANR-08-BLAN-0306-02) and funding from the RTB. G.D.P. was supported by EU Marie Curie (PIEF-GA-2009-237646) for part of the work. D.L. was supported by CEA-EUROTALENTS (PCOFUND-GA-2008-228664). Dr. M. Giffard is acknowledged for the synthesis of the TOTAPOL radical.

Abstract

original image

Ultra-fast: Substantial solid-state NMR sensitivity can be achieved using dynamic nuclear polarization and matrix-free sample preparation (that is, absence of solvent and cryoprotectant). This method avoids line-broadening, maximizes sample filling factor, and allows natural-abundance 2D 13C–13C dipolar correlation experiments to be carried out in tens of minutes. MW=microwaves.

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