Several recent papers have dealt with the modulation of protonated carbon response intensities in long-range heteronuclear 2D NMR chemical shift correlation spectra. Expressions describing the one-tend modulation of the response intensity of the C-3 methylene resonance of 6,7dimethoxy-3,4dihydroisoq
Repression of one-bond modulations in long-range heteronuclear 2D NMR spectra using a modified long-range optimized heteronuclear chemical shift correlation pulse sequence
โ Scribed by Andrew S. Zektzer; Boban K. John; Gary E. Martin
- Publisher
- John Wiley and Sons
- Year
- 1987
- Tongue
- English
- Weight
- 487 KB
- Volume
- 25
- Category
- Article
- ISSN
- 0749-1581
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โฆ Synopsis
A modified long-range heteronuclear chemical shift correlation pulse sequence which eliminates modulations of response intensity due to one-bond proton-carbon I'J(CH)] spin couplings is described. The 'decoupling' of one-bond modulation has been accomplished through the use of a bilinear rotational decoupling (BIRD) pulse of the type 90ยฐ,('H)-~-1800,('H)/1800,('3C~.r-900~,('H) midway through the second magnetization transfer delay, A*.
One-bond modulation of response intensities over a range of optimization values is demonstrated for the simple alkaloid norharmane when long-range optimization of the conventional heteronuclear chemical shift correlation pulse sequence is employed. The modified pulse sequence described eliminates one-bond modulations over the same range of optimization values. Slower modulations which arise due to long-range couplings other than that optimized for are present in both experiments.
Removal of the effects of one-bond modulation represents a potentially significant improvement in the utility of long-range heteronuclear chemical shift correlation experiments as a tool in spectral assignments and structure elucidation.
๐ SIMILAR VOLUMES
BIRD pulses have been shown to provide an effective means of decoupling ow-bond modulation of long-range response intensity. It is not possible to optimize the BIRD pulse effectively wben tbere is a range of one-bond coupling constants. To examine the effects of misoptimization of the fixed delays (