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note
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A typical reaction was as follows. Cumyl dithiobenzoate (0.28 g, 1.02 mmol) and AIBN (0.078 g, 0.47 mmol) were dissolved in a benzene (5.0 g) and styrene (5.0 g, 48 mmol) solution. An aliquot (0.2 g) of the solution was transferred to an ESR tube and oxygen removed by flushing with ultrahigh purity nitrogen for 10 min. The tube was sealed and transferred to the ESR cavity, which had been preheated to 90 °C.
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note
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The ESR spectra (including standards) were recorded on a Bruker EMX spectrometer in the X-band region, with the ER4102 cavity preheated to the reaction temperature. The magnetic field was modulated at 100 kHz, with amplitude between 0.1 and 0.5 mT, and a microwave power of 2 mW (well below saturation) was used. Spectra were recorded as single 1 or 5 min scans, and adjusted by subtraction of cavity scans under identical conditions.
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