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

作者：Equbal Asif; Basse Kristoffer; Nielsen Niels Chr^*

来源：Physical Chemistry Chemical Physics, 2016, 18(45): 30990-30997.

DOI：10.1039/c6cp06574k

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.

• 出版日期2016