A sensitive, high resolution magic angle turning experiment for measuring chemical shift tensor principal values

A sensitive, high-resolution 'FIREMAT' two-dimensional (2D) magic-angle-turning experiment is described that measures chemical shift tensor principal values in powdered solids. The spectra display spinning-sideband patterns separated by their isotropic shifts. The new method's sensiti...

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Bibliographic Details
Published in:Molecular physics 1998-12, Vol.95 (6), p.1113-1126
Main Authors: ALDERMAN, D. W., McGEORGE, GARY, HU, JIAN ZHI, PUGMIRE, RONALD J., GRANT, DAVID M.
Format: Article
Language:English
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Summary:A sensitive, high-resolution 'FIREMAT' two-dimensional (2D) magic-angle-turning experiment is described that measures chemical shift tensor principal values in powdered solids. The spectra display spinning-sideband patterns separated by their isotropic shifts. The new method's sensitivity and high resolution in the isotropic-shift dimension result from combining the 5π magic-angle-turning pulse sequence, an extension of the pseudo-2D sideband-suppression data rearrangement, and the TIGER protocol for processing 2D data. TPPM decoupling is used to enhance resolution. The method requires precise synchronization of the pulses and sampling to the rotor position. It is shown that the technique obtains 35 natural-abundance 13 C tensors from erythromycin in 19 hours, and high quality natural-abundance 15 N tensors from eight sites in potassium penicillin V in three days on a 400 MHz spectrometer.
ISSN:0026-8976
1362-3028
DOI:10.1080/00268979809483243