Approximately 20000 transients were collected (overnight) using a 30° pulse and a recycle delay of 1.5 s. 13C-NMR data were acquired at 75.47 MHz over 32K data points with a spectral width of 22700 Hz. 1H-NMR data were acquired at 300.13 MHz over 8K data points with a spectral width of 3400 Hz 32 transients were collected using a 20° pulse and a recycle delay of 3.3s. NMR data for 8 and 9 were acquired on a Bruker AM 300 spectrometer equipped with an Aspect 3000 computer, a variable temperature unit and a 5-mm broadband probe at 298 K. Chemical ionisation GC/MS data were obtained on a HP 5890 gas chromatograph interfaced to a HP 5980 mass spectrometer, using methane as the reagent gas. Electron impact GC/MS analysis was as reported previously 4. ![]() The detector temperature was 300☌ and the following oven temperature program was run: initial temperature 75☌ for 1 min, 20☌/min to 300☌, then 300☌ for 3 min. The injection temperature was held at 250☌ and used in the split mode with a split ratio of ~100:1. column with a 0.33 µm film thickness was used with He as carrier gas at a pressure of 150 kPa. The GC analysis was carried out on a Hewlett Packard 5880A GC equipped with a flame ionization detector.
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