This repository contains the experimental data discussed in the manuscript. Including, 1H NMR, 13C NMR (FID and PDF) and Mass Spectra for all the intermediates (A-H); probe 1; the hydroxylamine nitrone cyclic product; N-Methylhydroxylamine cyclic product; N,O,-BocHydroxylamine alkyne and N-Hydroxylamine alkyne. Fluorescence analysis data of probe 1 including the hydroxylamine titration curve; selectivity data against other hydroxylamines; amines and amino acids, Fluorescence intensity changes for probe 1 as a function of time with increasing concentrations of hydroxylamine (time drive) and cell images.