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Two microporous complexes, [Zn(TATAB)(OCH3)] ⋅2 H3O+ ( 1; TATAB=4,4′,4′′-[(1,3,5-triazine-2,4,6-triyl)tris(azanediyl)]tribenzoic acid), [Cu1.5(μ2-O)TATAB*] ( 2; TATAB*=4,4′-{[6-(dimethylamino)-1,3,5-triazine-2,4-diyl]bis(azanediyl)}dibenzoic acid) have been synthesized and characterized by elemental analysis, IR spectroscopy, UV absorption spectroscopy, and thermogravimetric analysis, and by powder XRD and single-crystal XRD analysis. Structural analyses revealed that complex 1 possesses a 3D porous framework with uncoordinated water molecules trapped in the pores; the dimensions of the channels are approximately 29.2×12.3 Å2. Complex 2 has a 3D microporous network structure. In addition, the surface photovoltage and photocatalytic activities were also studied. The photocatalytic properties of the two complexes were investigated by the decomposition of methylene blue under UV and visible-light irradiation. The results revealed that 2 possessea a higher photocatalytic activity than 1 under UV or visible-light irradiation. The potential semiconductor and dye degradation properties of complexes 1 and 2 may be widely applied in the fields of chemical semiconductors and environmental protection in the future. [ABSTRACT FROM AUTHOR]