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hncx2004

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The 400 MHz 1H-NMR spectra of all sample batches were analyzed on an AMX-II 600 MHz spectrometer (Bruker Instruments, Inc.), 32 scans were collected into 64 K data points over a spectral  width of 4789 Hz (12 ppm) with the transmitter offset at 5.00 ppm, yielding a digital resolution of 0.15 Hz per point. 1H-NMR high-temperature spectra at 353 K were measured at 300.13 MHz using a QMP probe. Thirty two scans were collected into 64 K data points over a spectral width of 6172.84 Hz (20.56 ppm). A flip angle of 30¡ã was used. The acquisition time was 5.31 s, followed by a relaxation delay of 1 s. An exponential line broadening window function of 0.3 Hz was used in the data processing. 13C-NMR spectra were recorded at 25 ¡ãC using a Bruker Avance 600 NH3 spectrometer operating at 14 T and equipped with a 5 mm broad-band probe. For the quantitative 13C-NMR study the following experimental parameters were used: 90 pulse width (14 s, ¨C3.0 dB), pulse delay of 38 s, spectral width of 21186.44 Hz (120 ppm), 64 K sampled points with 1.5 s to acquire them.

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xiaoqihu

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hncx2004

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hncx2004(½ð±Ò+5): 2010-02-28 22:06
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