Suppressing 1H Spin Diffusion in Fast MAS Proton Detected Heteronuclear Correlation Solid-State NMR Experiments

Venkatesh, Amrit; Hung, Ivan; Boteju, Kasuni C.; Sadow, Aaron D.; Gor’kov, Peter L.; Gan, Zhehong; Rossini, Aaron J.

doi:10.1016/j.ssnmr.2019.101636

Title: Suppressing ¹H Spin Diffusion in Fast MAS Proton Detected Heteronuclear Correlation Solid-State NMR Experiments

Journal Article · Wed Nov 13 00:00:00 EST 2019 · Solid State Nuclear Magnetic Resonance

DOI:https://doi.org/10.1016/j.ssnmr.2019.101636· OSTI ID:1668265

Venkatesh, Amrit ^[1]; Hung, Ivan ^[2]; Boteju, Kasuni C. ^[1]; Sadow, Aaron D. ^[1]; Gor’kov, Peter L. ^[2]; Gan, Zhehong ^[2]; Rossini, Aaron J. ^[1]

Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States). Dept. of Chemistry
Florida State Univ., Tallahassee, FL (United States). National High Magnetic Field Lab. (MagLab)

Fast magic angle spinning (MAS) and indirect detection by high gyromagnetic ratio (γ) nuclei such as proton or fluorine are increasingly utilized to obtain 2D heteronuclear correlation (HETCOR) solid-state NMR spectra of spin-1/2 nuclei by using cross polarization (CP) for coherence transfer. However, one major drawback of CP HETCOR pulse sequences is that ¹H spin diffusion during the back X→¹H CP transfer step results in relayed correlations. This problem is particularly pronounced for the indirect detection of very low-γ nuclei such as ⁸⁹Y, ¹⁰³Rh, ¹⁰⁹Ag and ¹⁸³W where long contact times on the order of 10 to 30 ms are necessary for optimal CP transfer. In this work, we propose two methods that eliminate relayed correlations and allow more reliable distance information to be obtained from 2D HETCOR NMR spectra. The first method uses Lee-Goldburg (LG) CP during the X→¹H back-transfer step to suppress ¹H spin diffusion. We determine LG conditions compatible with fast MAS frequencies (ν_rot) of 40- 95 kHz and show that ¹H spin diffusion can be efficiently suppressed at low effective radiofrequency (RF) fields (ν_1,eff << 0.5ν_rot) and also at high effective RF fields (ν_1,eff>> 2ν_rot). We describe modified Hartmann-Hahn LG-CP match conditions compatible with fast MAS and suitable for indirect detection of moderate-γ nuclei such as ¹³C, and low-γ nuclei such as ⁸⁹Y. The second method uses D-RINEPT (dipolar refocused insensitive nuclei enhanced by polarization transfer) during the X→¹H back-transfer step of the HETCOR pulse sequence. The effectiveness of these methods for acquiring HETCOR spectra with reduced relayed signal intensities is demonstrated with ¹H{¹³C} HETCOR NMR experiments on L-histidine•HCl•H₂O and ¹H{⁸⁹Y} HETCOR NMR experiments on an organometallic yttrium complex.

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Research Organization:: Ames Laboratory (AMES), Ames, IA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division; National Science Foundation (NSF); USDOE Office of Science (SC), Basic Energy Sciences (BES)

Contributing Organization:: Florida State Univ., Tallahassee, FL (United States). National High Magnetic Field Lab. (MagLab)

Grant/Contract Number:: AC02-07CH11358; DMR-1644779

OSTI ID:: 1668265

Alternate ID(s):: OSTI ID: 1693889

Report Number(s):: IS-J-10,108; DE-AC02-07CH11358; DE-AC02-07CH11358; DE-AC02-07CH11358; DE-AC02-07CH11358; DE-AC02-07CH11358; DE-AC02-07CH11358; DE-AC02-07CH11358

Journal Information:: Solid State Nuclear Magnetic Resonance, Vol. 105; ISSN 0926-2040

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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