This article contains the experimental data for the characterization of ∑3 boundaries in a cold deformed and annealed pure iron. Mentioned data are relevant to the research article " The inter-connections of ∑3 boundaries in pure iron" (Weiguo Wang, Song Chen, Gregory S. Rohrer, Wenzhe Chen, 2017) [1]. The characterization of ∑3 boundaries was performed through an integrated method including el...