Efficient Synthesis of Chiral Selenium Nano‐Hexagonal Prisms Through Chiral Crystallization for Enantioselective Photoreduction

Abstract Selenium with an asymmetric nanostructure exhibits fascinating chiral‐dependent properties. However, synthesis of chiral selenium nanomaterials with strong photocatalytic capabilities remains a formidable challenge. Herein, through a novel cysteine‐assisted crystallization strategy, chiral selenium nano‐hexagonal prisms (Se NHPs) with strong chiral optical activity and enantioselective photoreduction capability are constructed successfully for the first time. It is found that the chiral preference of Se NHPs is determined by the molecular chirality of cysteine during both seeds formation and crystallization stages. Homochiral combinations of these two steps amplified the circular dichroism (CD) signals of Se NHPs, while heterochiral combinations induce substantial suppression. Remarkably, enantioselective enhancement of the photoreduction efficiency of Se NHPs is achieved by introducing a chiral hole scavenger, tartaric acid. L‐tartaric acid selectively boosted the photoreduction efficiency of L‐type Se NHPs, and D‐tartaric acid exhibited a similar enhancement effect on D‐type Se NHPs. This work opens new avenues for the enantioselective crystallization of chiral nanomaterials and the improvement of enantioselective photocatalytic activity, paving the way for developing next‐generation chiral functional materials with enhanced optical performance.