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Two nickel(II) coordination polymers, formulated as {[Ni2(bix)2(tbta)2(H2O)4]·0.25H2O}n (1) and [Ni2(bix)(aip)2(H2O)2]n (2) [bix = 1, 4‐bis(imidazol‐1‐ylmethyl)benzene, H2tbta = tetrabromoterephthalic acid, H2aip = 5‐aminoisophthalic acid] were synthesized under hydrothermal conditions and structurally characterized by single‐crystal X‐ray diffraction methods, IR spectroscopy, TGA, and elemental analysis. Complex 1 exhibits a 2D (4, 4) layer with {44.62} topology. Complex 2 shows 2D (3, 4)‐connected 3,4L83 sheets, which are finally extended into an unusual (5, 6)‐connected 3D supramolecular network by classic hydrogen bond interactions. Fluorescence, UV/Vis diffuse reflection spectra, and catalytic properties of two complexes for the degradation of the methyl orange dye in a photo‐Fenton‐like process were investigated. [ABSTRACT FROM AUTHOR]