The molecular structure of free allyl radical was determined from high-temperature electron diffraction augmented with mass spectrometry. The free radicals, with 75% relative abundance, were produced by vacuum pyrolysis of 1,5-hexadiene at 960 O C in the diffraction experiment. The data are consistent with a planar symmetric geometry, C-C bond length (r,) 1.428 i 0.013 A, and C-C-C bond angle 124.6 i 3.4O.
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