Abstract
Rb[SbO(OH)4] was prepared under hydrothermal conditions at pH »10. The crystal structure was determined at ‐173 °C on basis of X‐ray data from a twinned crystal (P21, Z = 2, a = 5.6579(4), b = 7.2961(5), c = 5.6472(5) Å, β = 92.032(6)°; R1 = 0.0309, wR2 = 0.0903 for all data). In comparison with the crystal structures of other alkali hydroxidoantimonates(V), a novel polymeric anion 1µ[SbO2/2(OH)4/1]‐ is present, which is made up of [SbO2(OH)4] octahedra vertex‐sharing the trans‐aligned O atoms. All OH groups act as donor and acceptor groups of inter‐ and intra‐chain hydrogen bonds of moderate strengths. The Rb+ cations are situated between the chains and are bound to twelve O atoms from two O2− and ten OH groups. The dehydration process of Rb[SbO(OH)4] starts at »280 °C and yields RbSbO3 as the final product at 900 °C. Vibrational spectra (IR and Raman) show characteristic bands for the O−H and Sb−O(H) vibrations.
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