[Sb(12-Krone-4)2(CH3CN)][SbCl6]3 und [Bi(12-Krone-4)2(CH3CN)][SbCl6]3, die ersten Trikationen von Antimon(III) und Bismut(III) |
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Authors: | Ralf Garbe,Burkhard Vollmer,Bernhard Neumü ller,Jü rgen Pebler,Kurt Dehnicke |
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Abstract: | [Sb(12-Crown-4)2(CH3CN)][SbCl6]3 and [Bi(12-Crown-4)2(CH3CN)][SbCl6]3, first Trications of Antimony(III) and Bismuth(III) The crown ether complexes [M(12-crown-4)2(CH3CN)][SbCl6]3 with M = Sb and Bi are formed by the reaction of antimony trichloride and bismuth trichloride, respectively, with antimony pentachloride in acetonitrile solution in the presence of 12-crown-4. They form colourless, moisture sensitive crystals, which were characterized by X-ray structure determinations and by IR spectroscopy. The complex with M = Sb was also characterized by 121Sb Mössbauer spectroscopy. Both complexes crystallize isotypically in the orthorhombic space group Pbcn with four formula units per unit cell. M = Sb: 3 483 observed unique reflections, R = 0.038. M = Bi: 2 958 observed unique reflections, R = 0.036. The compounds consist of SbCl6? ions and trications [M(12-crown-4)2(CH3CN)]3+, in which the M3+ ions are ninefold coordinated by the eight oxygen atoms of the crown ether molecules and by the nitrogen atom of the acetonitrile molecule. The lone pair of the M3+ ions has no steric effect. |
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Keywords: | Crown ether complexes of Sb3+ and Bi3+ synthesis IR spectra 121Sb Mö ssbauer spectrum X-ray structures |
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