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Abstract
The reaction of Na2 SO4 and K2 SO4 with fuming sulfuric acid (65 % SO3 ) yielded colorless extremely sensitive crystals of Na[HS3 O10 ] (monoclinic; P21 /n (No. 14); Z=4; a=707.36(2), b=1378.56(4), c=848.10(3) pm; β=94.817(1)°; V=824.09(4)⋅106 pm3 ) and K[HS3 O10 ] (orthorhombic; Pccn (No. 56); Z=4; a=1057.16(3), b=807.81(2), c=897.57(2) pm; V=766.51(3)⋅106 pm3 ). The analogous rubidium compound Rb[HS3 O10 ] (orthorhombic; Pnma (No. 62); Z=4; a=891.43(3), b=1095.34(4), c=839.37(3) pm; V=819.58(5)⋅106 pm3 ) originates from the reaction of Rb2 CO3 and SO3 . All of the different structures contain the hitherto unknown anion [HS3 O10 ]- and are stamped by strong hydrogen bonds linking the anions either to dimers or chains. Theoretical investigations by DFT methods give further insight in the structural characteristics of [HS3 O10 ]- . The preparation of the [HS3 O10 ]- anion can be seen as an important milestone on our way to the still elusive polysulfuric acids.
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