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[Display omitted] • Fe/Co co-doped metal organic gels were prepared using solvothermal technique. • Synergistic effect of PMS activation and photocatalysis promotes ROS generation. • The synergistic system exhibits efficient degradation activity against NOR. • Intermediate identification and T.E.S.T calculations verify ecotoxicity fade. • The system exhibited antibacterial activity against E. coli and S. aureus. A strategically fabricated cobalt-doped iron-based metal–organic gel (CFM) synergistically promotes peroxymonosulfate (PMS) activation and visible light-induced photocatalysis to remove norfloxacin (NOR). Cobalt incorporation into the metal–organic gel significantly optimizes its electronic structure, leading to the exceptional performance of CFM in synergistically activating PMS, amplifying visible light absorption, and enhancing photoinduced charge separation efficiency. The Vis/50 %-CFM/PMS system enables a NOR removal rate of up to 96.8 % within 60 min and a total organic carbon (TOC) removal rate of 78.3 %, signifying excellent decontamination performance. Exhibiting robust mineralization potential, the Vis/CFM/PMS system has undergone comprehensive analysis of the intermediary degradation process using Density Functional Theory (DFT) calculations. The toxicity of degradation intermediates was assessed employing the quantitative structure–activity relationship (QSAR) model. In addition, the Vis/CFM/PMS system showed antibacterial effects against E. coli and S. aureus. This investigation furnishes a novel perspective toward developing innovative PMS activation photocatalyst coupling systems for environmental remediation. [ABSTRACT FROM AUTHOR]