The in situ electrical and NMR characterizations proceeded at the same time scale during the reaction. In addition, using the same concentration of the reagents in the same DCM/TMB solution, the mixed solution was separated into two parts: one for 1H NMR characterizations and the other for conductance monitoring (both of these measurements started after the reaction occurred). The single-molecule conductance evolution was observed as the reaction time increased, and each histogram was constructed with about 300 traces recorded from each set of data. The 1D conductance histograms were fitted by Gaussian function with peak differentiation, and the corresponding peak areas were integrated to determine the proportions of each specific molecular species. Thus, we could determine the proportion of the products at each time scale for further reaction rate evaluation. For further details, see the “In situ single-molecule conductance monitoring during the reaction” section in the Supplementary Materials. For the NMR spectroscopies characterized at each time scale, the concentration ratio of product/reactant can also be derived from the area integration of the H peaks of each species. For further details, see the “Kinetic information extracted from the in situ 1H NMR spectra” section in the Supplementary Materials.

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