An unusual O/F ordered d transition metal fluoroantimonite, namely, KSbMoOF, has been created by the cationic size effect of alkali metals. It features the largest birefringence of 0.220@550 nm among inorganic antimonites with a halogen element, which is an order of magnitude larger than the disordered ASbMoOF (A = Rb, Cs). These three new compounds exhibit two different structures, although all of the structures were made of [SbMoOF] chains formed by SbF square pyramids and MoOF octahedrons. A transparent single crystal of KSbMoOF with dimensions of 7.0 × 5.0 × 1.0 mm has been successfully grown by the aqueous solution volatilization method. The UV-vis-MIR transmission spectrum showed that KSbMoOF can display excellent transmittance in the range of 0.5-5.0 μm and 6.0-9.8 μm, indicating its application potential as a birefringent material in the mid infrared band. This work offers a fresh approach to the design and synthesis of mid infrared birefringent materials.
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