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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