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An organic–inorganic hybrid polyiodate, namely, [o‐C5H4NHOH]2[I7O18(OH)]⋅3 H2O (I), featuring a novel branched polyiodate chain has been obtained by evaporation method. [o‐C5H4NHOH]2[I7O18(OH)]⋅3 H2O (I) crystalizes in the polar space group Ia and features an [I7O18(OH)]∞2- branched polyiodate chain in which [I3O9]3− trimers are grafted on the same side of the one‐dimensional (1D) chain based on [I4O11(OH)]3− tetramers. The asymmetric organic amine groups are beneficial to the polymerization of iodate groups and inducing the formation of the non‐centrosymmetric (NCS) structure. Compound I exhibits a rather large Second‐Harmonic‐ Generation (SHG) signal of 8.5×KH2PO4 (KDP) upon 1064 nm laser radiation, a moderate band gap of 3.90 eV and a high laser‐induced‐damage‐threshold (LIDT) of 182.34 MW cm−2, hence it is a promising new SHG material. The relationship between the structures of the organic amine groups and the overall structures has been also analyzed. [ABSTRACT FROM AUTHOR]

The first alkali‐metal vanadium iodate fluoride, CsVO2F(IO3), with a novel 3D anionic framework, has been rationally designed and hydrothermally synthesized. The 3D [VO2F(IO3)]− framework in CsVO2F(IO3) is built from 0D Λ‐shaped cis‐[VO3F(IO3)2]4− polyanions via corner‐sharing of oxo anions and bridging of the iodate groups. CsVO2F(IO3) displays both a strong second‐harmonic generation (SHG) 1.1 times as strong as KTiOPO4 (KTP) under 2.05 μm laser radiation and high laser‐induced damage threshold (LIDT) of 107.9 MW cm−2. This work provides a new route to design SHG crystals with stable 3D anionic structures from low‐dimensional structural building units. [ABSTRACT FROM AUTHOR]

• NaMoO 3 (IO 3) is the first example of molybdenum(VI) iodate with 1D chain-like structure featuring a large birefringence (0.208@1064 nm). • Both 1D [MoO 3 (IO 3)]- anionic chain in NaMoO 3 (IO 3) and 3D [MoO 3 (IO 3)]- anionic framework in γ-KMoO 3 (IO 3) are assembled from 0D Λ-shaped cis -MoO 4 (IO 3) 2 units. • The polar 3D γ-KMoO 3 (IO 3) exhibits the largest SHG response (12 × KDP) among AMoO 3 (IO 3) family as well as a high LIDT value (52 × AGS). [Display omitted] Herein, we reported two alkali metal molybdenum(VI) iodates, namely, NaMoO 3 (IO 3) and γ-KMoO 3 (IO 3) with 1D and 3D [MoO 3 (IO 3)]− anionic architectures, respectively. The novel 1D chain in NaMoO 3 (IO 3) and the 3D network in γ-KMoO 3 (IO 3) are constructed by the 0D Λ-shaped cis -[MoO 4 (IO 3) 2 ]4− building units interconnected by bridging IO 3 − anions as well as the corner-sharing of oxo anions. Importantly, the polar γ-KMoO 3 (IO 3) exhibits a very large second-harmonic generation (SHG) effect of 12 × KH 2 PO 4 (KDP) under 1064 nm laser radiation, a high laser-Induced damage threshold value (52 × AgGaS 2), and a moderate birefringence of 0.087@1064 nm, whereas the centrosymmetric NaMoO 3 (IO 3) has a large birefringence of 0.208@1064 nm. This study further proves the useful route of exploring promising optical materials via assembling the 0D basic building units into higher dimensional anionic architectures. [ABSTRACT FROM AUTHOR]