The hydroxylation of cycloalkanes at 25 degrees C by the syringe pump addition of tert-alkyl hydroperoxides (10 and 1 equiv based on catalyst) to deoxygenated acetonitrile containing cycloalkanes (0.64 M) and 0.61 mM of the catalyst, [(Fe2O)-O-III(TPA)(2)(H2O)(2)](4+), is demonstrated to be a reaction which involves freely diffusing cycloalkyl radicals, i.e., free alkyl radicals.