Quantitative measurement of small through-hydrogen-bond and ‘through-space’1H-113Cd and1H-199Hg J couplings in metal-substituted rubredoxin fromPyrococcus furiosus
- 1 September 1992
- journal article
- research article
- Published by Springer Nature in Journal of Biomolecular NMR
- Vol. 2 (5) , 527-533
- https://doi.org/10.1007/bf02192814
Abstract
A method is described for measurement of small unresolvable heteronuclear J couplings. The method is based on quantitative analysis of a phase-purged heteronuclear spin-echo difference spectrum, and is demonstrated for measuring1H-113Cd and1H-199Hg J couplings in metal-substituted rubredoxin (Mr ∼ 5.4 kDa) fromPyrococcus furiosus. Couplings from cadmium to backbone amide protons that are hydrogen bonded to the Cys-S atoms directly bonded to Cd vary from smaller than 0.3 to 1.8 Hz; a ‘through-space’ coupling between Cd and the protons of an alanine methyl group was measured to be 0.3 Hz. Couplings to199Hg are significantly larger and fall in the 0.4–4 Hz range.Keywords
This publication has 8 references indexed in Scilit:
- Novel observation of NH--S(Cys) hydrogen-bond-mediated scalar coupling in cadmium-113 substituted rubredoxin from Pyrococcus furiosusJournal of the American Chemical Society, 1992
- Nuclear spin-spin coupling via nonbonded interactions. 7. Effects of molecular structure on nitrogen-fluorine couplingThe Journal of Organic Chemistry, 1992
- Solid-state mercury-199 and cadmium-113 NMR studies of mercury- and cadmium-thiolate complexes. Spectroscopic models for [Hg(SCys)n] centers in the bacterial mercury resistance proteinsJournal of the American Chemical Society, 1991
- Relaxation-allowed cross-peaks in two-dimensional N.M.R. correlation spectroscopyMolecular Physics, 1989
- Heteronuclear filters for two-dimensional proton NMR. Identification of the metal-bound amino acids in metallothionein and observation of small heteronuclear long-range couplingsJournal of the American Chemical Society, 1988
- Correlation of connected transitions by two-dimensional NMR spectroscopyThe Journal of Chemical Physics, 1986
- Weak satellite signals in high-resolution NMR spectra: Separating the wheat from the chaffJournal of Magnetic Resonance (1969), 1981
- NH---S hydrogen bonds in Peptococcus aerogenes ferredoxin, Clostridium pasteurianum rubredoxin, and Chromatium high potential iron protein.Proceedings of the National Academy of Sciences, 1975