Abstract
The crown ether complexes SbX3(15-crown-5) with X = F, Cl, Br, and I have been prepared by reactions of 15-crown-5 with the corresponding antimony trihalides in acetonitrile solutions. The compounds were characterized by IR spectroscopy as well as by 121Sb-Mössbauer spectroscopy. A method of orbital population analysis utilizing both Mössbauer isomer shifts and quadrupole coupling has been developed for Sb(III) antimony halides and their crown ether complexes. SbF3(15-crown-5) was also characterized by an X-ray structure determination: Space group P21/n, Z = 4, 3628 observed unique reflexions, R = 0.032. Lattice dimensions at 19 °C: a = 891.54(6), b = 1277.26(6), c = 1277.66(7) pm, β = 95.029(4)°. The complex has a molecular structure in which the antimony atom is surrounded by three F-atoms with mean bond lengths of 192.4 pm and by the five oxygen atoms of the crown ether molecule with mean bond lengths of 293.9 pm.
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