15N−H Bond Length Determination in Natural Abundance by Inverse Detection in Fast-MAS Solid-State NMR Spectroscopy
- 24 August 2002
- journal article
- research article
- Published by American Chemical Society (ACS) in Journal of the American Chemical Society
- Vol. 124 (37) , 10938-10939
- https://doi.org/10.1021/ja026657x
Abstract
A solid-state 15N−1H correlation NMR experiment is presented, which provides a substantial gain in signal sensitivity by 1H inverse detection under fast MAS conditions and allows for the precise determination of NH bond lengths via heteronuclear 1H−15N dipole−dipole couplings on samples naturally abundant in 15N. Pulsed-field gradients or, alternatively, radio frequency pulses ensure suppression of unwanted 1H signals. In this way, natural-abundance 15N−1H correlation NMR spectroscopy becomes feasible in the solid state with experiment times of a few hours. The dipole−dipole coupling constants are extracted from spinning sideband patterns generated by recently developed recoupling strategies. The information on 15N/1H chemical shifts and quantitative 15N−1H couplings can readily be combined in a single two-dimensional spectrum using a split-t1 approach.Keywords
This publication has 12 references indexed in Scilit:
- Investigation of an N···H hydrogen bond in a solid benzoxazine dimer by 1H–15N NMR correlation techniques under fast magic‐angle spinningMagnetic Resonance in Chemistry, 2001
- High-Resolution 1H NMR Spectroscopy in the Solid State: Very Fast Sample Rotation and Multiple-Quantum CoherencesJournal of Magnetic Resonance, 2001
- Inverse Detection and Heteronuclear Editing in 1H–15N Correlation and 1H–1H Double-Quantum NMR Spectroscopy in the Solid State under Fast MASJournal of Magnetic Resonance, 2001
- Sensitivity-Enhanced Static 15N NMR of Solids by 1H Indirect DetectionJournal of Magnetic Resonance, 2001
- Recoupled Polarization-Transfer Methods for Solid-State 1H–13C Heteronuclear Correlation in the Limit of Fast MASJournal of Magnetic Resonance, 2001
- Sensitivity Enhancement in Solid State 15N NMR by Indirect Detection with High-Speed Magic Angle SpinningJournal of Magnetic Resonance, 2000
- An Investigation of π−π Packing in a Columnar Hexabenzocoronene by Fast Magic-Angle Spinning and Double-Quantum 1H Solid-State NMR SpectroscopyJournal of the American Chemical Society, 1999
- Heteronuclear multidimensional NMR experiments for the structure determination of proteins in solution employing pulsed field gradientsPublished by Elsevier ,1999
- Enhancement of nuclear magnetic resonance signals by polarization transferJournal of the American Chemical Society, 1979
- Neutron diffraction study of L-histidine hydrochloride monohydrateActa Crystallographica Section B: Structural Science, Crystal Engineering and Materials, 1977