Constant-time 2D and 3D through-bond correlation NMR spectroscopy of solids under 60 kHz MAS

The Journal of Chemical Physics
Rongchun Zhang, Ayyalusamy Ramamoorthy

Abstract

Establishing connectivity and proximity of nuclei is an important step in elucidating the structure and dynamics of molecules in solids using magic angle spinning (MAS) NMR spectroscopy. Although recent studies have successfully demonstrated the feasibility of proton-detected multidimensional solid-state NMR experiments under ultrafast-MAS frequencies and obtaining high-resolution spectral lines of protons, assignment of proton resonances is a major challenge. In this study, we first re-visit and demonstrate the feasibility of 2D constant-time uniform-sign cross-peak correlation (CTUC-COSY) NMR experiment on rigid solids under ultrafast-MAS conditions, where the sensitivity of the experiment is enhanced by the reduced spin-spin relaxation rate and the use of low radio-frequency power for heteronuclear decoupling during the evolution intervals of the pulse sequence. In addition, we experimentally demonstrate the performance of a proton-detected pulse sequence to obtain a 3D (1)H/(13)C/(1)H chemical shift correlation spectrum by incorporating an additional cross-polarization period in the CTUC-COSY pulse sequence to enable proton chemical shift evolution and proton detection in the incrementable t1 and t3 periods, respectively. I...Continue Reading

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May 6, 2014·Journal of Magnetic Resonance·Rongchun Zhang, Ayyalusamy Ramamoorthy
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Dec 9, 2014·Journal of Magnetic Resonance·Rongchun ZhangAyyalusamy Ramamoorthy
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Citations

Jul 12, 2016·Solid State Nuclear Magnetic Resonance·Yusuke Nishiyama
Jun 17, 2016·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Rongchun ZhangAyyalusamy Ramamoorthy
May 9, 2021·Journal of Magnetic Resonance·Amrit VenkateshAaron J Rossini
Mar 30, 2017·Accounts of Chemical Research·Rongchun ZhangAyyalusamy Ramamoorthy
May 26, 2017·The Journal of Physical Chemistry. B·Rongchun ZhangAyyalusamy Ramamoorthy

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