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Homonuclear J-couplings and rotationally induced sideband enhancements in NMR spectra of rotating solids
Institution:1. Department of Chemistry, Massachusetts Institute of Technology, Cambridge, MA 02139, USA;2. Francis Bitter National Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, MA 02139, USA;3. Department of Chemistry, State University of New York at Stony Brook, Stony Brook, NY 11794, USA;4. Department of Chemistry, Lehigh University, Bethlehem, PA 18015, USA;1. Shanghai Engineering Research Center for Molecular Therapeutics and New Drug Development, School of Chemistry and Molecular Engineering, East China Normal University, Shanghai, 200062, China;2. NYU-ECNU Center for Computational Chemistry at NYU, Shanghai, China;3. Department of Chemistry, New York University, New York, 10003, United States;1. Department of Physics and Biophysics Interdepartmental Group, University of Guelph, Guelph, Ontario, Canada;2. Department of Chemistry, North Carolina State University, Raleigh, NC, USA;3. Bruker Biospin, Billerica, MA, USA;1. Center for Hyperpolarization in Magnetic Resonance, Magnetic Resonance, Department of Health Technology, Technical University of Denmark, Ørsteds Plads, 2800, Kgs. Lyngby, Denmark;2. Center for Hyperpolarization in Magnetic Resonance, Electromagnetic Systems Group, Department of Electrical Engineering, Technical University of Denmark, Ørsteds Plads, 2800, Kgs. Lyngby, Denmark;1. Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw, Poland;2. Department of Drug Chemistry, Wroclaw Medical University, Borowska 211, 50-556 Wroclaw, Poland;3. Department of Basic Medical Science, Wroclaw Medical University, Borowska 211, 50-556 Wroclaw, Poland
Abstract:We demonstrate direct detection of 13C-13C J-couplings in magic angle sample spinning NMR spectra despite the presence of the much larger homogeneous broadening caused by the homonuclear dipolar couplings. Carbon-carbon J-couplings were observed in doubly 13C-enriched samples of sodium acetate, glycine and glucose. The resolved J-coupling permits carbon-carbon connectivities to be established with standard two-dimensional techniques. Interesting spectral features are observed when the rotational sidebands of the coupled spins overlap: when a sideband from a dipolar-coupled pair approaches the centerband of its partner, a significant enhancement in sideband intensity is observed as well as small shifts in the resonance frequency.
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