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Abstract To achieve precise spatial control of donor–acceptor (D–A) stacking and optimize through‐space charge transfer (TSCT) for efficient photocatalysis, we develop a novel terpyridine bi‐functionalization strategy, which utilizes the dissymmetrical 6‐ and 4′‐functionalization of 2,2′:6′,2″‐terpyridine (tpy) scaffold with triphenyltriazine (acceptor) and triphenylamine (donor) units. Using this strategy, we designed and synthesized two ligands, L1 and L2 , differing by a single phenylene unit in length. Upon coordination with Zn(II), the D and A units in the resulting complexes S1 and S2 are precisely edited at the molecular level, giving rise to distinct stacking geometries: slip‐stacked S1 and co‐facially S2 . S2 significantly enhances TSCT, resulting in improved visible‐light absorption, prolonged charge carrier lifetime, superior charge separation efficiency and achieves a photocatalytic efficiency (2063 µmol g −1 h −1 ) for H 2 O 2 production that is twice that of S1 without the need for sacrificial agents. This work demonstrates the unique advantages of terpyridine bi‐functionalization strategy in constructing photocatalytic materials with tunable TSCT, providing new insights for the design and functional development of supramolecular systems.
Dai et al. (Thu,) studied this question.