Single crystals of two new iodide-iodates, Bi[IO]·AgI and Tb[IO]·AgI, are synthesized in hydrothermal systems. The anionic parts in both iodide-iodates are characterized as a complex charged framework of isolated IO umbrella-like groups and large Bi(Tb)-O polyhedra similar to those previously found in La[IO][IO](PbO). Broad channels along the c-axis contain compensators: (AgI) umbrella-like groups and additional Ag ions which form Ag tetrahedral clusters augmented with I halogen. New iodates possess significantly higher second-order nonlinear optical characteristics compared to the previously known lead-containing compounds REE[IO][IO](PbO), REE = La, Pr, Nd. The difference is related to the polar ordering of umbrella-like (AgI) groups in the channels in the new iodide-iodate. Additionally, planar-coordinated Ag atoms add three Ag atoms in umbrellas forming [AgI] polar clusters in the channels.
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