Pseudo-triple-resonance BIS-HMQC experiment for the 1H-detected measurement of couplings between rare spins
✍ Scribed by Ēriks Kupče; Edmunds Lukevics; Bernd Wrackmeyer
- Publisher
- John Wiley and Sons
- Year
- 1994
- Tongue
- English
- Weight
- 312 KB
- Volume
- 32
- Category
- Article
- ISSN
- 0749-1581
No coin nor oath required. For personal study only.
✦ Synopsis
Abstract
Improvement in the sensitivity and accuracy of the ^1^H‐detected experiment for measurement of coupling constants between rare spin‐1/2 nuclei X and Y is achieved if a bi‐selective (BIS) pulse is used to excite selectively protons coupled to Y, prior to the standard ^1^HX HMQC experiment (BIS‐HMQC). In the 2D spectrum even very small coupling constants J(X, Y) can be measured and the signs of J(X, Y) and J(Y ^1^H) can be compared. High‐quality 2D spectra were obtained using post‐acquisition binomial filters. The ^1^H^13^C^29^Si spin systems of the methoxy group in p‐trimethoxysilyltoluene [^2^J(^29^SiO^13^C) = 1.3 Hz] and of the diethylamino group in bis(diethylamino)dimethylsilane [^2^J(^29^SiN^13^C) = 2.5 Hz] serve for demonstrating the techniques.