PubMed Health⌕ Search
Home/Archive/PubMed

PubMed · 10378429

13C-1H dipolar recoupling under very fast magic-angle spinning using virtual pulses.

K Takegoshi·T Terao
View original source ↗Export metadata ↓

Abstract

A new solid-state NMR pulse sequence for recoupling 13C-1H dipolar interactions under magic-angle spinning is proposed, which works under a spinning speed of a few to several tens kilohertz. The sequence is composed of two different frequency switched Lee-Goldburg sequences, and the modulation of the spin part of the 13C-1H dipolar interaction is introduced by a virtual pulse sequence consisting of unitary operators connecting the rotating frame and the tilted rotating frame. When the cycle time of the spinning is equal to or twice the cycle time of the sequence, the 13C-1H dipolar interactions can be recoupled. The sequence is insensitive to experimental imperfections such as rf inhomogeneity or frequency offset, and the resulting lineshape can be represented by a simple analytical equation based on the zeroth-order average Hamiltonian. Experimental results for [2-(13)C] L-valine x HCl are reported.

Explore related subjects

Carbon IsotopesHydrogenMagnetic Resonance SpectroscopyValineJournal Article

Keep this discovery

Explore connections, maps & timelines

BibTeXRIS

K Takegoshi, T Terao. 1999. 13C-1H dipolar recoupling under very fast magic-angle spinning using virtual pulses.. https://doi.org/10.1016/s0926-2040(99)00005-3

Cite the original work for its findings. Save a collection to share your selection of sources.

KEEP EXPLORING

Related citations

PubMed2007

J-GFT NMR for precise measurement of mutually correlated nuclear spin-spin couplings.

G-matrix Fourier transform (GFT) NMR spectroscopy is presented for accurate and precise measurement of chemical shifts and nuclear spin-spin couplings correlated according to spin system. The new approach, named "J-GFT NMR", is based on a largely extended GFT NMR formalism and promises to have a broad impact on projection NMR spectroscopy. Specifically, constant-time J-GFT (6,2)D (HA-CA-CO)-N-HN was implemented for simultaneous measurement of five mutually correlated NMR parameters, that is, 15N backbone chemical shifts and the four one-bond spin-spin couplings 13Calpha-1Halpha, 13Calpha-13C', 15N-13C', and 15N-1HNu. The experiment was applied for measuring residual dipolar couplings (RDCs) in an 8 kDa protein Z-domain aligned with Pf1 phages. Comparison with RDC values extracted from conventional NMR experiments reveals that RDCs are measured with high precision and accuracy, which is attributable to the facts that (i) the use of constant time evolution ensures that signals do not broaden whenever multiple RDCs are jointly measured in a single dimension and (ii) RDCs are multiply encoded in the multiplets arising from the joint sampling. This corresponds to measuring the couplings multiple times in a statistically independent manner. A key feature of J-GFT NMR, i.e., the correlation of couplings according to spin systems without reference to sequential resonance assignments, promises to be particularly valuable for rapid identification of backbone conformation and classification of protein fold families on the basis of statistical analysis of dipolar couplings.

Carbon Isotopes↗
PubMed2007

Water source partitioning among trees growing on shallow karst soils in a seasonally dry tropical climate.

The sources of water used by woody vegetation growing on karst soils in seasonally dry tropical regions are little known. In northern Yucatan (Mexico), trees withstand 4-6 months of annual drought in spite of the small water storage capacity of the shallow karst soil. We hypothesized that adult evergreen trees in Yucatan tap the aquifer for a reliable supply of water during the prolonged dry season. The naturally occurring concentration gradients in oxygen and hydrogen stable isotopes in soil, bedrock, groundwater and plant stem water were used to determine the sources of water used by native evergreen and drought-deciduous tree species. While the trees studied grew over a permanent water table (9-20 m depth), pit excavation showed that roots were largely restricted to the upper 2 m of the soil/bedrock profile. At the peak of the dry season, the delta(18)O signatures of potential water sources for the vegetation ranged from 4.1 +/- 1.1 per thousand in topsoil to -4.3 +/- 0.1 per thousand in groundwater. The delta(18)O values of tree stem water ranged from -2.8 +/- 0.3 per thousand in Talisia olivaeformis to 0.8 +/- 1 per thousand in Ficus cotinifolia, demonstrating vertical partitioning of soil/bedrock water among tree species. Stem water delta(18)O values were significantly different from that of groundwater for all the tree species investigated. Stem water samples plotted to the right of the meteoric water line, indicating utilization of water sources subject to evaporative isotopic enrichment. Foliar delta(13)C in adult trees varied widely among species, ranging from -25.3 +/- 0.3 per thousand in Enterolobium cyclocarpum to -28.7 +/- 0.4 per thousand in T. olivaeformis. Contrary to initial expectations, data indicate that native trees growing on shallow karst soils in northern Yucatan use little or no groundwater and depend mostly on water stored within the upper 2-3 m of the soil/bedrock profile. Water storage in subsurface soil-filled cavities and in the porous limestone bedrock is apparently sufficient to sustain adult evergreen trees throughout the pronounced dry season.

Carbon Isotopes↗