Indirect detection of infinite-speed MAS solid-state NMR spectra

Perras, Frédéric A.; Venkatesh, Amrit; Hanrahan, Michael P.; Goh, Tian Wei; Huang, Wenyu; Rossini, Aaron J.; Pruski, Marek

doi:10.1016/j.jmr.2017.01.010

Indirect detection of infinite-speed MAS solid-state NMR spectra

Journal Article · Wed Jan 18 00:00:00 EST 2017 · Journal of Magnetic Resonance

DOI:https://doi.org/10.1016/j.jmr.2017.01.010· OSTI ID:1347897

Perras, Frédéric A. ^[1]; Venkatesh, Amrit ^[2]; Hanrahan, Michael P. ^[2]; Goh, Tian Wei ^[3]; Huang, Wenyu ^[2]; Rossini, Aaron J. ^[2]; Pruski, Marek ^[2]

Ames Lab., Ames, IA (United States)
Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States). Dept. of Chemistry
Iowa State Univ., Ames, IA (United States). Dept. of Chemistry

Heavy spin-1/2 nuclides are known to possess very large chemical shift anisotropies that can challenge even the most advanced magic-angle-spinning (MAS) techniques. Wide manifolds of overlapping spinning sidebands and insufficient excitation bandwidths often obfuscate meaningful spectral information and force the use of static, low-resolution solid-state (SS)NMR methods for the characterization of materials. In order to address these issues, we have merged fast-magic-angle-turning (MAT) and dipolar heteronuclear multiple-quantum coherence (D-HMQC) experiments to obtain D-HMQC-MAT pulse sequences which enable the rapid acquisition of 2D SSNMR spectra that correlate isotropic ¹H chemical shifts to the indirectly detected isotropic “infinite-MAS” spectra of heavy spin-1/2 nuclides. Furthermore, for these nuclides, the combination of fast MAS and ¹H detection provides a high sensitivity, which rivals the DNP-enhanced ultra-wideline SSNMR. The new pulse sequences were used to determine the Pt coordination environments in a complex mixture of decomposition products of transplatin and in a metal-organic framework with Pt ions coordinated to the linker ligands.

View Accepted Manuscript (DOE)

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

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1347897

Alternate ID(s):: OSTI ID: 1412960

Report Number(s):: IS-J--9222; PII: S1090780717300101

Journal Information:: Journal of Magnetic Resonance, Journal Name: Journal of Magnetic Resonance Journal Issue: C Vol. 276; ISSN 1090-7807

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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New frontiers for solid-state NMR across the periodic table: a snapshot of modern techniques and instrumentation Bryce, David L. Dalton Transactions, Vol. 48, Issue 23 https://doi.org/10.1039/c9dt01801h	journal	January 2019

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