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Hybrid organic–inorganic antimony halides have attracted increasing attention due to the non‐toxicity, stability, and high photoluminescence quantum yield (PLQY). To shed light on the structural factors that contribute to the high PLQY, five pairs of antimony halides with general formula A2SbCl5 and A2Sb2Cl8 are synthesized via two distinct methods and characterized. The A2SbCl5 type adopts square...
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