Adsorption-assisted photocatalysis is a new approach to control water pollution. A novel metal organic framework MIL 53(Fe–Cu) was formulated via a single-step solvothermal route. The newly developed MOF was successfully utilized to treat pharmaceutical waste–containing effluent using a combined mechanism of adsorption and photocatalytic degradation. The in-depth characterization of the MOF ensured its favorable physicochemical properties such as high surface area, porous nature, favorable functional groups on its surface, thermal stability and photocatalytic activity. Furthermore, PL spectroscopy proved that MIL 53(Fe–Cu) offers a reduced rate of electron–hole recombination. The newly developed MOF presented the highest adsorption uptake of 190.40 mg g⁻¹ for ciprofloxacin and a maximum degradation of 74.48 and 57.88% in the presence of UV and visible radiations, respectively. This experimental investigation confirms that novel MIL 53(Fe–Cu) outperforms the traditional materials in treating the pharmaceutical wastewater.