Abstract
AbstractThe reactions of KCl, [NH4]2[SO4], Rb2[CO3], and Cs2[CO3] with fuming sulfuric acid (65 % SO3) yielded colorless and moisture sensitive crystals of K[HS2O7] (monoclinic, P21/c (no. 14), Z = 4, a = 716.67(3) pm, b = 1043.57(4) pm, c = 828.78(3) pm, β = 107.884(1)°, V = 589.89(4) × 106 pm3), [NH4][HS2O7] (monoclinic, P21/c (no. 14), Z = 4, a = 729.29(1) pm, b = 1079.73(1) pm, c = 843.26(1) pm, β = 106.397(1)°, V = 637.01(1) × 106 pm3), Rb[HS2O7] (monoclinic, P21/c (no. 14), Z = 4, a = 724.49(2) pm, b = 1073.19(3) pm, c = 852.01(3) pm, β = 106.534(1)°, V = 635.06(3) × 106 pm3), and Cs[HS2O7] (triclinic, P (no. 2), Z = 2, a = 537.61(3) pm, b = 784.71(4) pm, c = 867.93(4) pm, α = 94.214(2)°, β = 103.138(2)°, γ = 105.814(2)°, V = 339.47(3) × 106 pm3). Colorless crystals of [NO][HS2O7] (monoclinic, P21/c (no. 14), Z = 4, a = 739.90(4) pm, b = 1048.00(5) pm, c = 830.97(4) pm, β = 106.985(2)°, V = 106.985(2) × 106 pm3) were obtained as a side product from the reaction of [NH4]2[Rh(NO2)4] with oleum (65 % SO3) in the ionic liquid [BMIm][OTf]. The crystal structures of K[HS2O7], [NH4][HS2O7], [NO][HS2O7], and Rb[HS2O7] show the [HS2O7]– ions linked into dimers by strong hydrogen bonds. Contrastingly, in the crystal structure of Cs[HS2O7] the [HS2O7]– ions are connected to infinite chains. Raman spectra were recorded for M[HS2O7] (M = K, Rb, Cs).
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