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Two acentric metal borates Ba3M2‐ [B3O6(OH)]2[B4O7(OH)2] (M=Al, Ga) have been made under hydrothermal conditions; the MO4 groups and two types of oxoboron cluster units interconnect to form a 3D porous layer with 9‐/14‐membered‐ring intersecting channels (see figure), showing a good second harmonic generation effect of about three times that of KH2PO4 (KDP).
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