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The photophysical tuning is reported for a series of tetraphenylphosphonium (TPP) metal halide hybrids containing distinct metal halides, TPP₂MX_n(MX_n=SbCl₅, MnCl₄, ZnCl₄, ZnCl₂Br₂, ZnBr₄), from efficient phosphorescence to ultralong afterglow. The afterglow properties of TPP⁺cations could be suspended for the hybrids containing low band gap emissive metal halide species, such as SbCl₅²⁻and MnCl₄²⁻, but significantly enhanced for the hybrids containing wide band gap non‐emissive ZnCl₄²⁻. Structural and photophysical studies reveal that the enhanced afterglow is attributed to stronger π–π stacking and intermolecular electronic coupling between TPP⁺cations in TPP₂ZnCl₄than in the pristine organic ionic compound TPPCl. Moreover, the afterglow in TPP₂ZnX₄can be tuned by controlling the halide composition, with the change from Cl to Br resulting in a shorter afterglow due to the heavy atom effect.

The photophysical tuning is reported for a series of tetraphenylphosphonium (TPP) metal halide hybrids containing distinct metal halides, TPP₂MX_n(MX_n=SbCl₅, MnCl₄, ZnCl₄, ZnCl₂Br₂, ZnBr₄), from efficient phosphorescence to ultralong afterglow. The afterglow properties of TPP⁺cations could be suspended for the hybrids containing low band gap emissive metal halide species, such as SbCl₅²⁻and MnCl₄²⁻, but significantly enhanced for the hybrids containing wide band gap non‐emissive ZnCl₄²⁻. Structural and photophysical studies reveal that the enhanced afterglow is attributed to stronger π–π stacking and intermolecular electronic coupling between TPP⁺cations in TPP₂ZnCl₄than in the pristine organic ionic compound TPPCl. Moreover, the afterglow in TPP₂ZnX₄can be tuned by controlling the halide composition, with the change from Cl to Br resulting in a shorter afterglow due to the heavy atom effect.

Zero‐dimensional (0D) organic metal halide hybrids, in which organic and metal halide ions cocrystallize to form neutral species, are a promising platform for the development of multifunctional crystalline materials. Herein we report the design, synthesis, and characterization of a ternary 0D organic metal halide hybrid, (HMTA)₄PbMn_0.69Sn_0.31Br₈, in which the organic cationN‐benzylhexamethylenetetrammonium (HMTA⁺, C₁₃H₁₉N₄⁺) cocrystallizes with PbBr₄²⁻, MnBr₄²⁻, and SnBr₄²⁻. The wide band gap of the organic cation and distinct optical characteristics of the three metal bromide anions enabled the single‐crystalline “host–guest” system to exhibit emissions from multiple “guest” metal halide species simultaneously. The combination of these emissions led to near‐perfect white emission with a photoluminescence quantum efficiency of around 73 %. Owing to distinct excitations of the three metal halide species, warm‐ to cool‐white emissions could be generated by controlling the excitation wavelength.

Zero‐dimensional (0D) organic metal halide hybrids, in which organic and metal halide ions cocrystallize to form neutral species, are a promising platform for the development of multifunctional crystalline materials. Herein we report the design, synthesis, and characterization of a ternary 0D organic metal halide hybrid, (HMTA)₄PbMn_0.69Sn_0.31Br₈, in which the organic cationN‐benzylhexamethylenetetrammonium (HMTA⁺, C₁₃H₁₉N₄⁺) cocrystallizes with PbBr₄²⁻, MnBr₄²⁻, and SnBr₄²⁻. The wide band gap of the organic cation and distinct optical characteristics of the three metal bromide anions enabled the single‐crystalline “host–guest” system to exhibit emissions from multiple “guest” metal halide species simultaneously. The combination of these emissions led to near‐perfect white emission with a photoluminescence quantum efficiency of around 73 %. Owing to distinct excitations of the three metal halide species, warm‐ to cool‐white emissions could be generated by controlling the excitation wavelength.