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The Oxidation of ReCl5 with Oleum: Synthesis and Crystal Structure of Re2O4Cl4(SO4)
Authors:Ulf Betke  Prof Dr Mathias S Wickleder
Institution:Carl von Ossietzky University of Oldenburg, Institute of Pure and Applied Chemistry, Carl‐von‐Ossietzky Stra?e 9–11, 26129 Oldenburg, Germany
Abstract:The reaction of ReCl5 and fuming sulfuric acid (25 % SO3) in a sealed glass tube at 200 °C led to red, needle shaped single crystals of Re2O4Cl4(SO4) (monoclinic, C2/c, a = 1501.8(2) pm, b = 1545.9(2) pm, c = 945.18(8) pm, β = 98.761(9)°, Z = 8). In the crystal structure the ReO2] moieties are linked by SO4]2– tetrahedra to chains along the 101] direction. Each sulfate ion connects four rhenium atoms, additional two chloride ions complete the octahedral coordination sphere of each rhenium atom according to $\rm^1_\infty$equation image ReO2/1Cl2/1(SO4)2/4].
Keywords:Sulfates  Oxide chlorides  Rhenium  Crystal structure  Oleum
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