Mesocrystals have the advantage of integrating the exploitable sizedependent properties of individual subunits and tuning the collective properties exhibited because of their interaction in aggregated states. In other words, nanomaterials can be designed by introducing this novel structure to improve their performances in specific fields. For example, the synthesis of iron oxide and manganese-doped zinc-sulfide mesocrystals was recently performed using a self-assembly process in an oil-in-water microemulsion method. [10] Due to structural benefits, superparamagnetic nature, and strong fluorescent signals, it was possible to achieve a tunable dynamic range of immunoassay with wash-free procedures. Alloyed PtNi mesocrystals were synthesized via a onepot solvothermal method. [11] They were used as efficient methanol oxidation catalysts owing to the structural benefits of mesocrystals, such as high surface-to-volume ratio, porous network, interconnected grains, and rigid framework. However, it has been challenging to take advantage of the versatility of the mesocrystals reported to date either because they consist of only a single component or because two types of building blocks were used for their assembly. Previous findings for efficient catalysts have caused an enormous influence on sustainable development. However, the practical application of catalysts in liquid phase reactions is still hampered due to high manufacturing and processing costs, agglomeration in aqueous solution, difficulties in catalyst separation, and recycling. [12-14] Catalysts have been retrieved through centrifugation or filtration methods, but these methods have limitations in terms of cost, efficiency, or generation of secondary waste; meanwhile, magnetic separation offers a robust, highly efficient, selective, and rapid catalyst separation tool. [15-17] To overcome these issues, heterogeneous photo-Fenton like catalysts have emerged as promising substitutes for magnetically recoverable catalysts. [18] Unfortunately, most of the photo-Fenton catalysts are injected into wastewater in the form of a powder that is not dispersed in water. If there is no external stimulus such as a physical stirring, light transmission efficiency to the floor where the catalysts exist would be very low. Therefore, this would be inefficient to purify large volumes of pollutants. Suitable magnetically recoverable photo-Fenton-like catalysts generate charge carriers by light absorption, inhibit Mesocrystals, consisting of small subunits, have gained research interests owing to their ability to simultaneously modify material-specific properties and interactions among subunits. However, despite these unique characteristics, most mesocrystals are composed of a single material, and there is a disjunction between academic discovery and practical application. In this study, the synthesis of multi-component mesocrystalline nanoparticles composed of Fe 3 O 4 , ZnFe 2 O 4 , and ZnO subunits using a polymerization induced heterogeneous nucleation method is reported. The str...