The dataset contains raw 1H NMR datasets from Agilent 600 MHz spectrometer. The series of spectra for two reactions are included: "mono-click" - Reaction between benzyl azide A and phenylacetylene B: 20 mM for both "bis-click" - Reaction between azide A and diyne D: 40 mM and 20 mM The reactions were monitored using an array of 1H NMR experiments, each with a single scan, acquired every 20 seconds for 5 hours. All NMR experiments were recorded on an Agilent 600 MHz with a DirectDrive 2 console and a room-temperature HCN probe. The spectral width was 9615.38 Hz, the pulse width was 9.1 us and the acquisition time was 1.70 s. Before initiating the reaction, the well-shimmed spectrum of the reaction mixture has been acquired. Similarly, after the reaction, the sample was shimmed, and the data were acquired.