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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 electron backscatter diffraction, stereology based five parameter analysis and crystallographic analysis. This method as formulated can determine the inter-connections of any type grain boundaries with fixed misorientation.