600mhz avance 1 spectrometer

The ¹⁹F NMR measurements were done at 20 °C using 3 mm tubes containing 200 μl of sample on a Bruker 600 MHz Avance I spectrometer equipped with a CP-QCI-F cryoprobe with Fluor Cryo-detection. ¹⁹F NMR experiments were done on control samples with compound 1 or compound 16 at 50 μM, 37.5 μM, 25 μM, 12.5 μM and 6.25 μM, in a 50 mM Hepes 100 mM NaCl buffer with a constant percentage (1%) of DMSO. The ¹⁹F titration experiments were carried out on samples containing 50 μM, 37.5 μM, 25 μM, 12.5 μM and 6.25 μM of compounds (1 and 16) with a constant enzyme concentration of 5 μM in the same buffer. The carrier frequency was set at −100 p.p.m. with a spectral window of 40 ppm, and 4,024 scans were recorded per sample, except for the 6.25 μM sample for which 12,288 scans were recorded.