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Exploiting the chirality transfer and amplification in the hierarchical chiral systems by the visible and accurate structures is still a challenge. Herein, a pair of homochiral metal‐organic frameworks (MOFs) DCF‐12 and LCF‐12 with high rigidity and high porosity are synthesized via reticular chemistry. Interestingly, these two enantiomers can act as nano‐containers, in which four chromophores, covering acridine, pyrene, 9,10‐Bis(phenylvinyl) anthracene (BPEA), and coronene can be introduced by in situ encapsulation. Importantly, the precise single crystal structures of all guest‐loaded MOFs by X‐ray diffraction technique can be obtained smoothly. It not only clearly reveals the chirality transfer from chiral host framework to achiral guest emitters through space chirality transfer, but also circularly polarized luminescence can be achieved and modulated through the synergistic effect. Extraordinarily, both pyrene@DCF‐12 and pyrene@LCF‐12 exhibit fascinating multi‐color tunable room temperature phosphorescence (RTP) and dynamic circularly polarized luminescence. Besides, the RTP quantum yields of pyrene@DCF‐12 and pyrene@LCD‐12 are high up to 75.39% and 73.43%, which exceeds most of that of RTP materials. These results demonstrate that chiral MOFs can serve as an accurate platform to investigate the mechanism of chirality transfer and amplification and to prompt the development of CPL‐active materials.
A series of host‐guest chiral metal‐organic frameworks (MOFs) are synthesized, and the structures of guests@MOFs can be obtained by single crystal X‐ray diffraction. It provides accurate models to reveal the chirality transfer from chiral frameworks to achiral guests. Circularly polarized luminescence and room temperature phosphorescence can be regulated through synergistic effects. These results provide an accurate approach to developing chiral optical materials.