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Can proton-proton recoupling in fully protonated solids provide quantitative, selective and efficient polarization

Nghia Tuan Duong¹, Sreejith Raran-Kurussi², Yusuke Nishiyama³

¹NMR Science and Development Division, RIKEN SPring-8 Center, and Nano-Crystallography Unit, RIKEN-JEOL Collaboration Center, Yokohama, Kanagawa 230-0045, Japan.

Journal of Magnetic Resonance (San Diego, Calif. : 1997)

|July 4, 2020

Summary

This study compares broadband and selective proton recoupling sequences for solid-state NMR. It evaluates their efficiency in transferring polarization and measuring distances in dense proton networks.

Area of Science:

Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy
Materials science
Chemical physics

Background:

Dipolar recoupling sequences are crucial for probing nuclear spin proximity in solid-state NMR.
Traditionally, these sequences targeted rare spins (e.g., 13C, 15N) due to weak couplings and broad chemical shifts.
Protons (1H) possess strong dipolar couplings and narrow chemical shifts, necessitating specialized recoupling strategies.

Purpose of the Study:

To evaluate the performance of various broadband and selective 1H-1H recoupling sequences.
To assess their efficiency in polarization transfer within dense proton networks.
To explore their utility in measuring 1H-1H distances for structural characterization.

Main Methods:

Theoretical analysis of recoupling Hamiltonians.
Numerical simulations of spin dynamics.
Experimental validation using L-histidine.HCl.H2O at 71.43 kHz MAS.
Comparison of finite pulse RFDR (fp-RFDR), BASS-SD, SOCP, and SERP sequences.

Main Results:

Demonstrated distinct advantages and disadvantages of each recoupling sequence.
Evaluated selectivity and efficiency of 1H-1H polarization transfers.
Provided experimental data supporting theoretical and simulation findings.

Conclusions:

Rationalized the selection criteria for appropriate 1H-1H recoupling sequences in fully protonated solids.
Highlighted the importance of sequence choice for accurate structural information.
Contributed to the advancement of solid-state NMR methodologies for complex protonated systems.

Keywords:

(1)H-(1)H distances (1)H-(1)H recoupling Broadband recoupling Fast MAS Selective recoupling

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