Highly efficient F-19 heteronuclear decoupling in solid-state NMR spectroscopy using supercycled refocused-CW irradiation

Asif Equbal, Kristoffer Basse, Niels Christian Nielsen

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Abstract

We present heteronuclear F-19 refocused CW (rCW) decoupling pulse sequences for solid-state magic-angle- spinning NMR applications. The decoupling sequences have been designed specifically to ensure suppression of the pertinent C-13-F-19 dipolar coupling interactions while simultaneously suppressing strong anisotropic chemical shift as well as homonuclear F-19-F-19 dipolar coupling effects as typically present in perfluorated compounds. In an extensive numerical and experimental analysis using a rigid, organic solid as a model compound, it becomes evident that the supercycled rCW schemes markedly improve the decoupling efficiency, leading to substantial enhancements in resolution and sensitivity when compared to previous state-of-the-art methods. Furthermore, considerable gains in robustness toward rf mismatch as well as offset in the radio-frequency carrier frequency are observed, all of which clearly render the new rCW schemes the methods of choice for 19F decoupling in rigid, fluorinated compounds - which is further supported by a Floquet-based theoretical analysis.

Original languageEnglish
JournalPhysical Chemistry Chemical Physics
Volume18
Issue45
Pages (from-to)30990-30997
Number of pages8
ISSN1463-9076
DOIs
Publication statusPublished - 2016

Keywords

  • NUCLEAR-MAGNETIC-RESONANCE
  • AMYLOID FIBRILS
  • ROTATING SOLIDS
  • SPIN
  • SIMULATION
  • FREQUENCY
  • DIPOLAR
  • ASSIGNMENT
  • SEQUENCE
  • SIMPSON

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