Hydrothermal Synthesis of Two Cationic Bismuthate Clusters: An Alkylenedisulfonate Bridged Hexamer, [Bi<sub>6</sub>O<sub>4</sub>(OH)<sub>4</sub>(H<sub>2</sub>O)<sub>2</sub>][(CH<sub>2</sub>)<sub>2</sub>(SO<sub>3</sub>)<sub>2</sub>]<sub>3</sub> and a Rare Nonamer Templated by Triflate, [Bi<sub>9</su
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This paper reports the synthesis, characterization, and application of two cationic bismuthate clusters by anion templating. The compounds were synthesized under mild hydrothermal treatment and characterized by powder and single-crystal X-ray diffraction, infrared spectroscopy, and thermogravimetric analysis. The first material consists of a cationic hexanuclear bismuthate cluster octahedral in geometry and linked by 1,2-ethanedisulfonate molecules. This structure is thermally stable to about 235 °C. In the second compound, discrete cationic nonanuclear bismuthate clusters interact electrostatically with trifluoromethanesulfonate anions to pack into a nearly layered assembly. The material undergoes a transformation to Bi2O3 upon loss of the triflate groups at about 385 °C. Both materials demonstrate the use of sulfonate groups for the anion-directed assembly of these rare cationic inorganic structures. The application of the 3D octahedral bismuth cluster material toward acidic heterogeneous catalysis is also reported.
