To conduct NMR analysis, samples were prepared by dissolving each sample in 650 μL of DMSO-d6 (Sigma Aldrich®) to obtain the concentration of 5 mg/ml then transferred to 5 mm 7″ NMR tubes. J-resolved and proton (1H NMR) experiments were performed using a Bruker® AVIII HD 500 (11.7 T) and the spectra were processed using MestReNova x64 software (version 14.1.2).
The data acquisition followed the parameters used in the previous work developed by Sampaio et al. (2016) (link) using 16 scans in the pre-saturation pulse sequence for one-dimensional (1D) proton spectra (1H NMR) and 32 scans and 64 increments per scan for two-dimensional (2D) 1H−1H J-resolved (J-res) NMR spectra; data points widths of 3.56 kHz for F2 (chemical shift axis) and 50 Hz for F1 (spin-spin coupling constant axis). The solvent signal was suppressed by the selective pre-saturation method.
The data acquisition followed the parameters used in the previous work developed by Sampaio et al. (2016) (link) using 16 scans in the pre-saturation pulse sequence for one-dimensional (1D) proton spectra (1H NMR) and 32 scans and 64 increments per scan for two-dimensional (2D) 1H−1H J-resolved (J-res) NMR spectra; data points widths of 3.56 kHz for F2 (chemical shift axis) and 50 Hz for F1 (spin-spin coupling constant axis). The solvent signal was suppressed by the selective pre-saturation method.
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