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Oxychalcogenides have been drawn much attention to be explored as nonlinear optical (NLO) materials in recent years. To date, all the NLO oxychalcogenides crystallize in low dimensional structures. Herein, a new oxysulfide K2Ba0.5Ga9O2S13 was obtained via three‐dimensional (3D) {[Ga9O2S13]3–}∞ polyanionic framework. As the first oxychalcogenide with 3D NLO‐acitve polyanionic framework, K2Ba0.5Ga9O...
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