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The first example of a rare-earth metal nitrate-selenite nonlinear optical (NLO) crystal, Gd(NO3)(Se2O5)·3H2O (1), was synthesized by hydrothermal reaction. This compound crystallizes in the noncentrosymmetric space group P212121, and its structure features two-dimensional (2D) [Gd(NO3)(Se2O5)]∞ layers, extending to a pseudo-3D framework linked by hydrogen bonds. 1 exhibits a phase-matchable SHG efficiency about 0.2 times that of KH2PO4 (KDP) and a large laser damage threshold of 236.26 MW cm-2. The UV-Vis-NIR diffuse reflectance spect
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