3 mm gradient probe

NMR experiments were carried out on a Varian INOVA 500 MHz (¹H) spectrometer with 3 mm gradient probe at 25–50°C with acetone internal reference (2.225 ppm for ¹H and 31.45 ppm for ¹³C), using standard pulse sequences gCOSY (gradient COrrelation SpectroscopY), TOCSY (Total Correlation Spectroscopy) (mixing time 120 ms), NOESY (Nuclear Overhauser Effect Spectroscopy) (mixing time 300 ms), gHSQC (gradient Heteronuclear Single Quantum Coherence), and gHMBC (gradient Heteronuclear Multiple Bond Coherence) (100 ms long range transfer delay). AQ time was kept at 0.8–1 sec for H-H correlations and 0.25 sec for HSQC. 256 increments were acquired for t1 in all 2D spectra, except 512 for gCOSY.

NMR experiments were carried out on a Varian INOVA 500 MHz (¹H) spectrometer with 3 mm gradient probe at 25°C with acetone internal reference (2.225 ppm for ¹H and 31.45 ppm for ¹³C) using standard pulse sequences DQCOSY, TOCSY (mixing time 120 ms), ROESY (mixing time 500 ms), HSQC and HMBC (100 ms long range transfer delay). AQ time was kept at 0.8–1 s for H-H correlations and 0.25 s for HSQC, 256 increments was acquired for t1. For ¹H-³¹P HMQC H-P coupling was set to 10 Hz.