skip to main content

DOE PAGESDOE PAGES

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

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.
Authors:
 [1] ;  [2] ;  [2] ;  [3] ;  [2] ;  [2] ;  [2]
  1. Ames Lab., Ames, IA (United States)
  2. Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States). Dept. of Chemistry
  3. Iowa State Univ., Ames, IA (United States). Dept. of Chemistry
Publication Date:
Report Number(s):
IS-J-9222
Journal ID: ISSN 1090-7807; PII: S1090780717300101; TRN: US1800090
Grant/Contract Number:
AC02-07CH11358
Type:
Accepted Manuscript
Journal Name:
Journal of Magnetic Resonance
Additional Journal Information:
Journal Volume: 276; Journal Issue: C; Journal ID: ISSN 1090-7807
Publisher:
Elsevier
Research Org:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Org:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; ultra-fast MAS; magic-angle-turning; D-HMQC; Platinum NMR; metal-organic-framework
OSTI Identifier:
1347897
Alternate Identifier(s):
OSTI ID: 1412960

Perras, Frédéric A., Venkatesh, Amrit, Hanrahan, Michael P., Goh, Tian Wei, Huang, Wenyu, Rossini, Aaron J., and Pruski, Marek. Indirect detection of infinite-speed MAS solid-state NMR spectra. United States: N. p., Web. doi:10.1016/j.jmr.2017.01.010.
Perras, Frédéric A., Venkatesh, Amrit, Hanrahan, Michael P., Goh, Tian Wei, Huang, Wenyu, Rossini, Aaron J., & Pruski, Marek. Indirect detection of infinite-speed MAS solid-state NMR spectra. United States. doi:10.1016/j.jmr.2017.01.010.
Perras, Frédéric A., Venkatesh, Amrit, Hanrahan, Michael P., Goh, Tian Wei, Huang, Wenyu, Rossini, Aaron J., and Pruski, Marek. 2017. "Indirect detection of infinite-speed MAS solid-state NMR spectra". United States. doi:10.1016/j.jmr.2017.01.010. https://www.osti.gov/servlets/purl/1347897.
@article{osti_1347897,
title = {Indirect detection of infinite-speed MAS solid-state NMR spectra},
author = {Perras, Frédéric A. and Venkatesh, Amrit and Hanrahan, Michael P. and Goh, Tian Wei and Huang, Wenyu and Rossini, Aaron J. and Pruski, Marek},
abstractNote = {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.},
doi = {10.1016/j.jmr.2017.01.010},
journal = {Journal of Magnetic Resonance},
number = C,
volume = 276,
place = {United States},
year = {2017},
month = {1}
}