ABSTRACT Large, high‐quality single crystals are essential for uncovering intrinsic photophysics in organic–inorganic hybrid metal halides (OIHMs), yet their growth remains challenging. We report a solvent‐engineered strategy that provides controlled solubility and a wide metastable zone, enabling the growth of centimetre‐sized C 24 H 20 P‐MnBr crystals, the largest reported Mn‐based OIHM crystal to date. These bulk crystals reveal, for the first time, an intrinsic blue emission (λ em = 430 nm, τ ≈ 228 ps) originating from the organic cation, and polarized spectroscopy confirms directional energy transfer to Mn 2 + , revising the excited‐state dynamics of this system. The crystals exhibit excellent scintillation performance with a light yield of 66,468 photons/MeV and an energy resolution of 44.1% at 50 keV. Our solvent‐based approach is general and applicable to other hybrid halides, demonstrating that large single crystals are crucial for uncovering complex photophysics and advancing radiation‐detection devices.
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