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Cations that can regulate the configuration of anion group are greatly important but regularly unheeded. Herein, the structural transformation from 2D CS to 3D noncentrosymmetric (NCS, which is the prerequisite for second‐order NLO effect) is rationally designed to newly afford two sulfides LiMGa8S14 (M = Rb/Ba, 1; Cs/Ba, 2) by introducing the smallest alkali metal Li+ cation into the interlamination...
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