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A novel strategy for the synthesis of zinc thioporphyrazine nanospheres is presented. The uniform spheres were fabricated through a polymerization reaction without using any template or emulsifier, which result from the covalent links between zinc tetra(2,3-bis(pentenylthio)porphyrazine (ZnPz) possessing eight long flexible chains in periphery and each with one terminal olefin group. A possible mechanism to explain the self-assembly of ZnPz nanospheres was also illuminated through monitoring nanosphere formation by means of transmission electron microscopy (TEM). More importantly, ZnPz nanospheres can effectively activate dioxygen in aqueous media under simulated sunlight irradiation, and showed significantly improved photocatalytic activity for the degradation of Rhodamine B (RhB) as compared to monomeric ZnPz. Furthermore, the reactive oxygen species derived from ZnPz nanospheres under light irradiation were determined by electron paramagnetic resonance (EPR) technology, indicating that singlet oxygen ([Formula: see text]O[Formula: see text] and hydroxyl radical (•OH) are the major reactive oxygen species. The facile synthetic methodology and the enhanced photocatalytic performance of the ZnPz nanospheres endow this novel material with the potential of being an efficient biomimetic photocatalyst for wastewater treatment.