Affiliation:
1. Carl von Ossietzky University Oldenburg, Institute for Chemistry, Carl-von-Ossietzky Straße 9-11, 26129 Oldenburg, Germany
2. Technische Universität Dresden, Anorganische Chemie 2, Bergstrasse 66, 01069 Dresden, Germany
Abstract
Abstract
[bmim][HPy][S2O7] [monoclinic, P21/n, Z = 4, a = 825.78(2), b = 1545.30(3), c = 1410.80(3) pm, β = 104.726(1)°, V = 1741.16(7) Å3] was obtained as a side product in the reaction of GeCl4, oleum (65% SO3), and the pyridine (Py) complex Py·SO3 in the ionic liquid 1-butyl-3-methylimidazolium hydrogensulfate, [bmim][HSO4], at 50 °C. Charge compensation of the disulfate ion is achieved by the counterions pyridinium, [HPy]+, and 1-butyl-3-methylimidazolium, [bmim]+. The crystal structure shows alternating layers of [bmim]+ cations on one hand and [HPy]+ cations and disulfate anions on the other hand. Pyridinium disulfate, [HPy]2[S2O7] [orthorhombic, P212121, Z = 4, a = 801.35(1), b = 1257.62(2), c = 1357.22(3) pm, V = 1367.80(4) Å3] was formed unexpectedly in the reaction of Eu2O3 and Py·SO3 in pyridine. The crystal structure exhibits a layer-like arrangement of disulfate and pyridinium moieties in the ab plane. In both compounds, the disulfate groups are essentially uncoordinated allowing for a detailed inspection of “naked” S2O7
2– ions.