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Fast MAS total through-bond correlation spectroscopy.

E H Hardy1, R Verel, B H Meier

  • 1Laboratory for Physical Chemistry, ETH-Zentrum, 8092 Zurich, Switzerland. edha@nmr.phys.chem.ethz.ch

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|March 10, 2001
PubMed
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New total through-bond correlation spectroscopy (TOBSY) sequences were developed for fast magic angle spinning (MAS) solid-state NMR. These robust sequences enable effective broadband excitation for improved spectral assignments in complex molecules.

Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) Spectroscopy
  • Spectroscopic Method Development
  • Chemical Physics

Background:

  • Total through-bond correlation spectroscopy (TOBSY) is crucial for spin system identification in solid-state NMR.
  • Existing TOBSY sequences often face limitations with fast magic angle spinning (MAS) conditions.
  • Developing robust and effective sequences for fast MAS is essential for analyzing complex materials.

Purpose of the Study:

  • To design and develop novel mixing sequences for total through-bond correlation spectroscopy (TOBSY) in solids.
  • To optimize these sequences for broadband excitation and robustness under fast magic angle spinning (MAS) conditions.
  • To facilitate the assignment of resonances in solid-state NMR spectra.

Main Methods:

Related Experiment Videos

  • Utilized lowest order average Hamiltonian theory to identify sequences targeting the homonuclear isotropic J interaction.
  • Employed numerical simulations to evaluate sequence performance as a function of MAS frequency.
  • Experimental validation using a uniformly (13)C-labeled decapeptide at 20 kHz MAS.

    • Main Results:

    • Successfully developed new TOBSY sequences suitable for fast MAS.
    • Demonstrated broadband and effective excitation properties of the new sequences.
    • Obtained an experimental TOBSY spectrum of a decapeptide, enabling (13)C resonance assignment.

    Conclusions:

    • The developed TOBSY sequences are effective for fast MAS solid-state NMR.
    • These sequences provide a robust method for obtaining total through-bond correlations.
    • The new methodology aids in the assignment of (13)C resonances and spin systems in complex samples.