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Two UV inorganic yttrium selenite optical materials, namely, Y(HSeO 3)(SeO 3)(H 2 O)·(H 2 O) (1) and Y 2 (SeO 3) 2 (SeO 4)(H 2 O) 2 ·(H 2 O) 0.75 (2), have been synthesized successfully by hydrothermal reactions. Of these, Y 2 (SeO 3) 2 (SeO 4)(H 2 O) 2 ·(H 2 O) 0.75 (2) is a new mixed valent selenium oxide containing Se(IV) and Se(VI) cations simultaneously. Y(HSeO 3)(SeO 3)(H 2 O)·(H 2 O) (1) shows a 3D structure composed of 2D yttrium selenite layers linked by O−H···O bonds. Y 2 (SeO 3) 2 (SeO 4)(H 2 O) 2 ·(H 2 O) 0.75 (2) exhibits a 3D structure composed of 2D yttrium selenite layers connected by SeO 4 tetrahedron. Y(HSeO 3)(SeO 3)(H 2 O)·(H 2 O) (1) crystallized in a chiral space group P 2 1 2 1 2 1 and could display a moderate SHG intensity about 0.7 times of the commercial KH 2 PO 4 (KDP). Its powder laser damage threshold quantity was estimated to be 120.2 MW/cm2, which is about 46.2 times that of AGS (2.6 MW/cm2). UV–vis–NIR spectra reflectance spectra showed that these solids are wide band gap compounds with Eg of 5.5 and 5.1 eV respectively. Theoretical calculations disclosed that Y(HSeO 3)(SeO 3)(H 2 O)·(H 2 O) (1) is an indirect band gap structures and its bandgaps is determined by O and Se atoms. [Display omitted] • Y(HSeO 3)(SeO 3)(H 2 O)•(H 2 O) is a UV NLO material in pure selenite compounds with balanced properties. • Y(HSeO 3)(SeO 3)(H 2 O)•(H 2 O) exhibits a moderate SHG intensity, wide band gap, large LIDT and moderate birefringence. • Y 2 (SeO 3) 2 (SeO 4)(H 2 O) 2 •(H 2 O) 0.75 is a new mixed valent selenium oxide containing Se(IV) and Se(VI) cations simultaneously. [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]