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Two-dimensional pulsed TRIPLE at 95 GHz

Epel1, Goldfarb

  • 1Department of Chemical Physics, Weizmann Institute of Science, Rehovot, 76100, Israel.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|September 2, 2000
PubMed
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A new two-dimensional (2D) TRIPLE resonance experiment simplifies complex Electron Nuclear Double Resonance (ENDOR) spectra. This method aids in assigning signals to paramagnetic centers and determining hyperfine coupling signs.

Area of Science:

  • Magnetic Resonance Spectroscopy
  • Quantum Chemistry
  • Solid-State Physics

Background:

  • The one-dimensional (1D) pulsed TRIPLE resonance experiment is a modification of the Davies ENDOR experiment.
  • It utilizes an additional radiofrequency (RF) pi-pulse during the mixing time to generate a TRIPLE spectrum.
  • The difference TRIPLE spectrum isolates ENDOR lines within the same M(S) manifold.

Purpose of the Study:

  • To extend the 1D TRIPLE resonance experiment into two dimensions (2D).
  • To develop a method for simplifying and assigning signals in congested spectra from multiple paramagnetic centers.
  • To determine the relative signs of hyperfine couplings.

Main Methods:

  • Implementation of a 2D TRIPLE resonance experiment by sweeping frequencies of two RF pulses.

Related Experiment Videos

  • Application of the 2D experiment at high magnetic fields (W-band, 94.9 GHz).
  • Analysis of homonuclear and heteronuclear 2D TRIPLE spectra on Cu(2+)-doped l-histidine.

    • Main Results:

    • The 2D TRIPLE experiment effectively resolves signals from different paramagnetic centers and their M(S) manifolds.
    • Connectivities in the 2D spectra allow straightforward assignment of (1)H, (14)N, and (35)Cl signals to specific Cu(2+) centers.
    • Relative signs of hyperfine couplings were determined.

    Conclusions:

    • The 2D TRIPLE resonance experiment is a powerful tool for analyzing complex paramagnetic systems.
    • This technique significantly aids in spectral assignment and understanding hyperfine interactions.
    • The method is particularly advantageous at high magnetic fields for separating signals.