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Rb 3 [H(HSO 4 ) 2 ][S 2 O 7 ] (monoclinic,  C 2/ c  (no. 15),  a= 1638.75(6),  b= 768.52(3),  c= 1187.88(4) pm,  β= 106.805(2)°,  V= 1432.14(9)·10 6  pm,  Z= 4) was obtained from the reaction of Rb 2 [CO 3 ] (99.9%, not dried, 150 mg, 0.6 mmol) with neat SO 3  in a torch-sealed glass ampoule. The remaining quantity of water in the starting material was obviously sufficient to lead to an H-containing substance. The structure shows the unprotonated disulfate anion [S 2 O 7 ] 2−  adjacent to the hydrogenium- bis -hydrogensulfate anion [H(HSO 4 ) 2 ] −  with the central hydrogen atom located close to a center of inversion.

zeitschrift für naturforschung b

Hydrogenium- bis -hydrogensulfate anions adjacent to [S 2 O 7 ] 2−  in Rb 3 [S 2 O 7 ][H(HSO 4 ) 2 ]: a structural evidence of the increasing acidity of polysulfuric acids with growing chain length