Disulfates from Low Temperature Synthesis in Ionic Liquids: (C5H6N)(3)Sm(S2O7)(3) and (C5H6N)Bi(S2O7)(2)

作者:Weiz Alexander; Bruns Joern; Wickleder Mathias S*
来源:European Journal of Inorganic Chemistry, 2014, 2014(1): 172-177.
DOI:10.1002/ejic.201301055

摘要

The reactions of Bi(NO3)(3)center dot 5H(2)O or Sm(NO3)(3)center dot 6H(2)O with oleum (65% SO3 in conc. H2SO4) and the pyridine (Py) complex Py center dot SO3 in the ionic liquid 1-butyl-3-methylimidazolium hydrogen sulfate, [bmim][HSO4], yielded single crystals of (C5H6N)Bi(S2O7)(2) and (C5H6N)(3)Sm(S2O7)(3), respectively. In (C5H6N)(3)Sm(S2O7)(3) the Sm3+ cations are ninefold coordinated by oxygen atoms in the form of a tricapped trigonal prism. The oxygen atoms belong to six chelating and six monodentate disulfate units. The anions connect the Sm3+ ions to chains according to (1)(infinity)[Sm(S2O7)(6/2)](3-) along the crystallographic c-axis. In (C5H6N)Bi(S2O7)(2) the two crystallographic independent Bi3+ cations are in a distorted square-prismatic oxygen coordination of eight oxygen atoms belonging to four chelating disulfate units. The connection of the Bi3+ ions leads to a corrugate layer according to (2)(infinity)[Bi(S2O7)(4/2)](-). In both compounds charge compensation is achieved by pyridinium cations (C5H6N)(+), which are tilted towards each other and packed in a layered arrangement between the anionic units. Thermoanalytical investigations reveal the sesquioxide Sm2O3 as a residual product for the decomposition of (C5H6N)(3)Sm(S2O7)(3).

  • 出版日期2014-1