Abstract
The solvothermal reaction of RbCl, boric acid, and chlorosulfuric acid yielded Rb[B(SO 4 ) 2 ]. The crystal structure of Rb[B(SO 4 ) 2 ] (tetragonal, P 4/ ncc, Z = 4, a = 9.1823(3) Å, c = 7.4559(5) Å, V = 628.64(6) Å) is isotypical to the previously published borosulfates A [B(SO 4 ) 2 ] ( A = K , Ag) and exhibits 1D anionic chains of vertex‐connected (SO 4 )‐ and (BO 4 )‐tetrahedra. The product has been obtained phase pure according to powder X‐ray diffraction and subsequent Rietveld refinement.

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