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Fast multidimensional NMR spectroscopy by spin‐state selective off‐resonance decoupling (SITAR)
Author(s) -
Keller Rochus,
Grace Christy Rani R.,
Riek Roland
Publication year - 2006
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.1818
Subject(s) - chemistry , decoupling (probability) , nuclear magnetic resonance spectroscopy , spectroscopy , resonance (particle physics) , spin (aerodynamics) , nuclear magnetic resonance , solid state nuclear magnetic resonance , atomic physics , stereochemistry , quantum mechanics , physics , thermodynamics , control engineering , engineering
Spin‐state selective off‐resonance decoupling (SITAR) is applied to the amide proton‐to‐nitrogen‐to‐alpha‐carbon correlation (HNCA) triple‐resonance experiment by measuring the 15 N chemical shift during the acquisition simultaneously with the 1 H chemical shift. The simultaneous detection of both 1 H and 15 N chemical shifts in SITAR reduces the dimensionality of the HNCA‐type experiment from three dimensions to two dimensions with a 15 N chemical shift resolution of ∼0.4 ppm. This enables the recording of triple‐resonance experiments in several minutes. SITAR is furthermore applied to the amide proton‐to‐nitrogen‐to‐alpha‐carbon‐and‐beta‐carbon correlation (HNCACB) triple‐resonance experiment and the 15 N‐resolved [ 1 H, 1 H]‐nuclear Overhauser enhancement spectroscopy (NOESY) experiment with similar success. The accompanied peak crowding and chemical shift degeneracy of the amide protons in the SITAR two‐dimensional (2D) spectra, which are inherent properties of pseudo‐dimensional experiments, are resolved by local correlation of the two sub‐spectra. With this procedure a 13 C 1 H strip for each 15 N 1 H moiety is generated resulting in a three‐dimensional (3D) strip list known from the conventional 3D spectra. The quality of the strip list in terms of peak crowding and chemical shift degeneracy is comparable to their corresponding 3D counterparts. An analysis‐software within the CARA package is presented, which generates, visualizes and manages the SITAR spectra, the corresponding strip lists and the assignment process. Copyright © 2006 John Wiley & Sons, Ltd.