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Synthese,Kristallstrukturen und 121Sb-Mößbauer-Spektren von [SbBr3(15-Krone-5)], [SbBr2Me(15-Krone-5)] und [SbBr2Ph(15-Krone-5)]
Authors:Michael Schfer  Jürgen Pebler  Kurt Dehnicke
Institution:Michael Schäfer,Jürgen Pebler,Kurt Dehnicke
Abstract:Synthesis, Crystal Structure, and 121Sb-Mössbauer Spectra of SbBr3(15-Crown-5)], SbBr2Me(15-Crown-5)], and SbBr2Ph(15-Crown-5)] The compounds SbBr3(15-crown-5)] ( 1 ), SbBr2Me(15-crown-5)] ( 2 ), SbBr2Ph(15-crown-5)] ( 3 ), and SbCl2Me(15-crown-5)] ( 4 ) are formed by the reaction of 15-crown-5 with SbBr3, SbBr2Me, SbBr2Ph, and SbCl2Me, respectively, in toluene solution at ?40°C. The complexes were characterized by IR spectroscopy, 121Sb-Mössbauer spectroscopy, 1–3 as well as by X-ray structure determinations.
  • 1 : Space group P212121, Z = 4, 1735 observed, independent reflections, R = 0.050, Lattice dimensions at ?65°C: a = 787.03(7); b = 1313.0(2); c = 1619.3(2) pm.
  • 2 : Space group Pca21, Z = 8, 2730 observed, independent reflections, R = 0.050, Lattice dimensions at ?65°C: a = 1308.2(2); b = 1611.8(2); c = 1640.5(3) pm.
  • 3 : Space group P21/n, Z = 4,2458 observed, independent reflections, R = 0.040, Lattice dimensions at ?60°C: a = 900.3(3); b = 1390.6(6); c = 1618.5(7) pm, β = 96.32(3)°.
The complexes 1–3 have molecular structures, in which the antimony atoms are surrounded by the five oxygen atoms of the crown ether molecule and by three ligands Br3, Br2CH3, Br2Ph, respectively.
Keywords:Antimony crown ether complexes  preparation  crystal structure  IR  121Sb-Mö  ssbauer spectra
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