Determination of the chemical shift tensor anisotropy and asymmetry of strongly dipolar coupled protons under fast MAS

Kobayashi, Takeshi; Perras, Frédéric A.; Nishiyama, Yusuke

doi:10.1016/j.ssnmr.2021.101743

Determination of the chemical shift tensor anisotropy and asymmetry of strongly dipolar coupled protons under fast MAS

Journal Article · Sat Jun 12 00:00:00 EDT 2021 · Solid State Nuclear Magnetic Resonance

DOI:https://doi.org/10.1016/j.ssnmr.2021.101743· OSTI ID:1798968

^[1]; Perras, Frédéric A. ^[1]; ^[2]

Iowa State Univ., Ames, IA (United States)
Inst. of Physical and Chemical Research (RIKEN), Wako (Japan); JEOL Resonance Inc., Tokyo (Japan)

Orientationally-dependent interactions such as dipolar coupling, quadrupolar coupling, and chemical shift anisotropy (CSA) contain a wealth of spatial information that can be used to elucidate molecular conformations and dynamics. To determine the sign of the chemical shift tensor anisotropy parameter (δ_aniso), both the |m| = 1 and |m| = 2 components of the CSA need to be symmetry allowed, while the recoupling of the |m| = 1 term is accompanied with the reintroduction of homonuclear dipolar coupling components. Therefore, previously suggested sequences which solely recouple the |m| = 2 term cannot determine the sign a ¹H's δ_aniso in a densely-coupled network. Here, we demonstrate the CSA recoupling of strongly dipolar coupled ¹H spins using the $$Cn^1_n (90_{0}360_{180}540_{0}360_{180}90_{0})$$ sequence. This pulse scheme recouples both the |m| = 1 and |m| = 2 CSA terms but the scaling factors for the homonuclear dipolar coupling terms are zeroed. Consequently, the sequence is sensitive to the sign of δ_aniso but is not influenced by homonuclear dipolar interactions.

View Accepted Manuscript (DOE)

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

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division; JSPS KAKENHI; JST-Mirai Program

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1798968

Report Number(s):: IS-J--10,508

Journal Information:: Solid State Nuclear Magnetic Resonance, Journal Name: Solid State Nuclear Magnetic Resonance Vol. 114; ISSN 0926-2040

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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