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Metal Assisted Synthesis of Cationic Sulfidobismuth Cubanes in Ionic Liquids.

ABSTRACT: Bi2 S3 was dissolved in the presence of either AuCl/PtCl2 or AgCl in the ionic liquids [BMIm]Cl???xAlCl3 (BMIm=1-n-butyl-3-methylimidazolium; x=4-4.3) through annealing the mixtures at 180 or 200?°C. Upon cooling to room temperature, orange, air-sensitive crystals of [BMIm](Bi4 S4 )[AlCl4 ]5 (1) or Ag(Bi7 S8 )[S(AlCl3 )3 ]2 [AlCl4 ]2 (2) precipitated, respectively. 1 did not form in the absence of AuCl/PtCl2 , suggesting an essential role of the metal cations. X-ray diffraction on single-crystals of 1 revealed a monoclinic crystal structure that contains (Bi4 S4 )4+ heterocubanes and [AlCl4 ]- tetrahedra as well as [BMIm]+ cations. The intercalation of the ionic liquid was confirmed via solid state NMR spectroscopy, revealing unusual coupling behavior. The crystal structure of 2 consists of (Bi7 S8 )5+ spiro-dicubanes, [S(AlCl3 )3 ]2- tetrahedra triples, isolated [AlCl4 ]- tetrahedra, and heavily disordered silver(I) cations. No cation ordering took place in 2 upon slow cooling to 100?K.

SUBMITTER: Knies M 

PROVIDER: S-EPMC7874255 | biostudies-literature | 2021 Feb

REPOSITORIES: biostudies-literature

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Metal Assisted Synthesis of Cationic Sulfidobismuth Cubanes in Ionic Liquids.

Knies Maximilian M   Groh Matthias F MF   Pietsch Tobias T   Lê Anh Mai M   Ruck Michael M  

ChemistryOpen 20201019 2

Bi<sub>2</sub> S<sub>3</sub> was dissolved in the presence of either AuCl/PtCl<sub>2</sub> or AgCl in the ionic liquids [BMIm]Cl ⋅ xAlCl<sub>3</sub> (BMIm=1-n-butyl-3-methylimidazolium; x=4-4.3) through annealing the mixtures at 180 or 200 °C. Upon cooling to room temperature, orange, air-sensitive crystals of [BMIm](Bi<sub>4</sub> S<sub>4</sub> )[AlCl<sub>4</sub> ]<sub>5</sub> (1) or Ag(Bi<sub>7</sub> S<sub>8</sub> )[S(AlCl<sub>3</sub> )<sub>3</sub> ]<sub>2</sub> [AlCl<sub>4</sub> ]<sub>2</sub>  ...[more]

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