An in-depth account of the effects of homonuclear couplings and multiple heteronuclear couplings is given for a recently published technique for 1 H-13 C dipolar correlation in solids under very fast MAS, where the heteronuclear dipolar coupling is recoupled by means of REDOR -pulse trains. The meth
Recoupled Polarization Transfer Heteronuclear 1H–13C Multiple-Quantum Correlation in Solids under Ultra-fast MAS
✍ Scribed by Kay Saalwächter; Robert Graf; Hans W. Spiess
- Publisher
- Elsevier Science
- Year
- 1999
- Tongue
- English
- Weight
- 91 KB
- Volume
- 140
- Category
- Article
- ISSN
- 1090-7807
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✦ Synopsis
A new approach for high-resolution solid-state heteronuclear multiple-quantum MAS NMR spectroscopy of dipolar-coupled spin-1 2 nuclei is introduced. The method is a heteronuclear chemical shift correlation technique of abundant spins, like 1 H with rare spins, like 13 C in natural abundance. High resolution is provided by ultra-fast MAS and high magnetic fields, high sensitivity being ensured by a direct polarization transfer from the abundant protons to 13 C. In a rotor-synchronized variant, the method can be used to probe heteronuclear through-space proximities, while the heteronuclear dipolar coupling constant can quantitatively be determined by measuring multiple-quantum spinning-sideband patterns. By means of recoupling, even weak heteronuclear dipolar interactions are accessible. The capabilities of the technique are demonstrated by measurements on crystalline L-tyrosine hydrochloride salt.
📜 SIMILAR VOLUMES
Signal enhancement in heteronuclear correlation spectra as well as signal selection in 1 H experiments can be achieved through inverse, i.e., 1 H, detection in the solid state under fast MAS conditions. Using recoupled polarization transfer (REPT), a heteronuclear 1 H-15 N single-quantum correlation