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- Proton and HMBC experiments were performed in CDCl3 using the AM500. The carbon and DEPT experiments were performed in CDCl3 using the AM300. The proton experiment was obtained with a spectral width of 10000 Hz and an observation pulse of 2.8 μsec (π/4). The carbon and DEPT experiments were obtained with a spectral width of 18518.5 Hz and π/2 and π/4 carbon pulses. The HMBC data sets were collected with spectral widths of 5000Hz (F2) and 29411 Hz (F1). Proton π/2 pulse was 7.5 μsec and the carbon π/2 pulse was 10 μsec. The first data set was optimized for long range couplings equal to 5Hz (D2 = 3.57 ms and D4 = 100 ms). The second data set was optimized for long range couplings equal to 7Hz (D2 = 3.57 ms and D4 = 70 ms). The data sets were collected with 2048 data points in F2 and and 512 increments, 32 scans each, in F1. The data sets were zero filled to 2K × 1K matrix and then transformed in both dimensions with a π/2 shifted sine squared function
- The full characterizations of compounds 6 and 7 were first reported in reference 13.