Determination of accurate

Fluorination is a versatile and valuable modification for numerous systems, and (19)F NMR spectroscopy is the premier method for their structural characterization. (19)F chemical shift anisotropy is a sensitive probe of structure and dynamics, even though (19)F chemical shift tensors have been reported for only a handful of systems to date. Here, we explore γ-encoded R-symmetry based recoupling sequences for the determination of (19)F chemical shift tensors in fully protonated organic solids at high, 60–100 kHz MAS frequencies. We show that the performance of (19)F-RNCSA experiments improves with increasing MAS frequencies, and that (1)H decoupling is required to determine accurate chemical shift tensor parameters. In addition, these sequences are tolerant to B(1)-field inhomogeneity making them suitable for a wide range of systems and experimental conditions.