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Borosulfates are a rapidly expanding class of silicate analogue materials, where the structural diversity is expected to be at least as large as known for silicates. However, borosulfates with cross-linking of the anionic network into two or even three dimensions are still very rare. Herein, we present two new representatives with phyllosilicate analogue topology. Through solvothermal reactions of ZnO and MnCl2∙4H2O with boric acid in oleum (65% SO3), we obtained single-crystals of Mn[B2(SO4)4] (monoclinic, P21/n, Z = 2, a = 8.0435(4), b = 7.9174(4), c = 9.3082(4) A, β = 110.94(1)°, V = 553.63(5) A3) and Zn[B2(SO4)4] (monoclinic, P21/n, Z = 2, a = 7.8338(4), b = 8.0967(4), c = 9.0399(4) A, β = 111.26(1)°, V = 534.36(5) A3). The crystal structures reveal layer-like anionic networks with alternating vierer- and zwolfer-rings formed exclusively by corner-linked (SO4)- and (BO4)-tetrahedra.

M[B2(SO4)4] (M = Mn, Zn)—Syntheses and Crystal Structures of Two New Phyllosilicate Analogue Borosulfates