Dipolar Heteronuclear Correlation Solid-State NMR Experiments between Half-Integer Quadrupolar Nuclei: The Case of 11B–17O

Dorn, Rick W.; Paterson, Alexander L.; Hung, Ivan; Gor’kov, Peter L.; Thompson, Austin J.; Sadow, Aaron D.; Gan, Zhehong; Rossini, Aaron J.

doi:10.1021/acs.jpcc.2c02737

Title: Dipolar Heteronuclear Correlation Solid-State NMR Experiments between Half-Integer Quadrupolar Nuclei: The Case of ¹¹B–¹⁷O

Journal Article · Thu Jul 07 00:00:00 EDT 2022 · Journal of Physical Chemistry. C

DOI:https://doi.org/10.1021/acs.jpcc.2c02737· OSTI ID:1877378

Dorn, Rick W. ^[1];

^[2];

^[3]; Gor’kov, Peter L. ^[3]; Thompson, Austin J. ^[4]; Sadow, Aaron D. ^[4];

^[3];

^[1]

Ames Lab., and Iowa State Univ., Ames, IA (United States)
Ames Lab., Ames, IA (United States); Univ. of Wisconsin, Madison, WI (United States)
National High Magnetic Field Lab. (NHMFL), Tallahassee, FL (United States)
Iowa State Univ., Ames, IA (United States)

With 73% of all NMR-active nuclei being quadrupolar, there is great interest in the development of NMR experiments that can probe the proximity of quadrupolar spins. Here, pulse sequences for magic-angle spinning (MAS) ¹¹B–¹⁷O resonance-echo saturation-pulse double-resonance (RESPDOR) and dipolar heteronuclear multiple quantum correlation (D-HMQC) solid-state NMR experiments were investigated. In these pulse sequences, rotational-echo double-resonance (REDOR) recoupling was used with central transition (CT)-selective π-pulses applied to either the ¹¹B or ¹⁷O spins to recouple ¹¹B–¹⁷O dipolar interactions. ¹¹B{¹⁷O} RESPDOR experiments on ¹⁷O-enriched boric acid and benzene diboronic acid showed that application of dipolar recoupling on the ¹¹B channel yielded more signal dephasing than when recoupling is applied on the ¹⁷O channel; however, short effective ¹¹B transverse relaxation time constants (T₂') hinder the acquisition of dephasing curves out to long recoupling durations. Application of REDOR recoupling to ¹⁷O spins was found to produce significant dephasing without compromising the ¹¹B T₂'. Comparison of experimental ¹¹B{¹⁷O} RESPDOR curves to those of numerical simulations enabled the ¹⁷O isotopic enrichment to be estimated. 2D ¹¹B{¹⁷O} D-HMQC spectra were recorded with either ¹¹B or ¹⁷O REDOR recoupling under a variety of radio frequency field conditions. Lastly, 2D ¹¹B{¹⁷O} and ²³Na{¹⁷O} D-HMQC spectra of an ¹⁷O-enriched sodium borate glass were acquired to demonstrate the practical application of these heteronuclear correlation experiments to probe structural connectivity between two quadrupolar spins. Importantly, the high-field 2D ¹¹B–¹⁷O D-HMQC NMR spectrum revealed two unique ¹⁷O sites correlating to 4-coordinate BO₄ (^[4]B), which were attributed to the ^[3]B–O–^[4]B and ^[4]B–O–^[4]B bridging O atoms. Furthermore, the heteronuclear correlation experiments outlined here should be applicable to a variety of quadrupolar spin pairs.

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

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

Grant/Contract Number:: AC02-07CH11358; CHE-1900393; NSF/DMR-1644779; DMR-1039938; DMR-0603042

OSTI ID:: 1877378

Report Number(s):: IS-J 10,848; 1916809

Journal Information:: Journal of Physical Chemistry. C, Vol. 126, Issue 28; ISSN 1932-7447

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Title: Dipolar Heteronuclear Correlation Solid-State NMR Experiments between Half-Integer Quadrupolar Nuclei: The Case of 11B–17O

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Title: Dipolar Heteronuclear Correlation Solid-State NMR Experiments between Half-Integer Quadrupolar Nuclei: The Case of ¹¹B–¹⁷O