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A new copper (II) coordination complex formulated as [Cu (dipic)(phen)(2‐MePy)]. 2H2O (1) where phen = 1, 10‐phenanthroline, dipic2− = pyridine‐2,6‐dicarboxylato and 2‐MePy = 2‐methyl pyrrole was synthesized through a simple and environment‐friendly reaction under ultrasound irradiation. Also, complex 1 was synthesized by hydrothermal process at 120 °C for 3 days. The corresponding structure of complex 1 was characterized by elemental analysis, atomic absorption spectroscopy (AAS), inductively coupled plasma (ICP), conductivity measurement, Fourier‐transform infrared spectroscopy (FT‐IR), Raman spectroscopy, ultraviolet–visible spectroscopy (UV–Vis), thermal gravimetric analysis (TGA), differential thermal analysis (DTA), scanning electron microscopy (SEM), vibrating sample magnetometer (VSM) and fluorescence. The crystal structure of the hydrothermally synthesized complex was characterized by single crystal X‐ray diffraction (SC‐XRD(, which revealed a triclinic structure. In the remainder of this study, the Cu2O nanoparticles have been prepared via thermal decomposition of hydrothermal and ultrasound complexes and characterized by ICP, FT‐IR, powder X‐ray diffraction (XRD), SEM and N2 adsorption/desorption. Adsorption and visible‐light‐driven photocatalytic capabilities of two synthetic Cu2O were investigated in the removal of MB from water. The result showed that the synthesized catalysts have good catalytic activity and the photocatalytic degradation is more effective in dye removal of MB compared with the adsorption.