Files are structured on three nested level depending on i) chemical system, ii) individual experiment and iii) irradiation time. Each final folder contains the acquisition and processing original file from the spectrometer. i) The nomenclature of the chemical systems corresponds to those described in the manuscript (Chem. Commun., 2020,56, 10461-10464). ii) For each system we performed 9 individual experiments, three triplicates, with an NMR tube for each one of them. iii) Each tube was irradiated for incremental periods of time and the NMR spectra acquired. Each folder contains the data corresponding to a different irradiation time, labeled as follows: · 1 -> Irradiation time = 0 s · 2 -> Irradiation time = 15 s · 3 -> Irradiation time = 1 min · 4 -> Irradiation time = 2 min · 5 -> Irradiation time = 7 min · 6 -> Irradiation time = 17 min · 7 -> Irradiation time = 22 min · 8 -> Irradiation time = 32 min