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1Author    Michael Plate, Gerlinde Frenzen, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstrukturen der ionischen Kronenetherkomplexe [TiCl3(15-Krone-5)(CH3CN)l[SbCl6l und | V Cl(OH)( 18-Krone-6)(CH3CN)2] [SbCl6l * V2(18-Krone-6 * CH3CN) Synthesis and Crystal Structures of the Ionic Crown Ether Complexes [TiCl3( 15-Crown-5)(CH3CN)][SbCl6] and [VCl(OH)( 18-Crown-6)(CH3C N )2][SbCl6] ■ 'A( 18-Crown-6 * C H 3CN)  
 Abstract    The title compounds were prepared by the reaction o f titanium tetrachloride with 15-crown-5 and antimony pentachloride, and by the reaction o f vanadium trichloride with 18-crown-6 and antimony pentachloride in the presence o f traces o f water in acetonitrile solution, respectively. The complexes were characterized by IR spectroscopy and by X-ray structure determinations. [TiCl3(15-crown-5)(CH1CN)][SbCl6]: Space group Pnma, Z = 4, 1355 observed unique reflec­ tions, R = 0.035. Lattice dim ensions at -8 0 °C: a = 1987(1), b = 1742.2(6), c = 111.0(2) pm. The com pound consists o f SbCl6~ anions and cations [TiCl3(15-crown-5)(CH3C N)]+, in which the titanium atom is coordinated octahedrally by three chlorine atom s in facial arrangement, by the nitrogen atom o f the acetonitrile m olecule, and by two oxygen atom s o f the crown ether molecule. [VCl(OH)(18 -crown-6)(C H 3C N)2][SbCl6] ■ 'A(18-crow n-6 • C H 3 CN); Space group P I, 3936 observed unique reflections, R = 0.014. Lattice dim ensions at -8 0 °C: a = 1194.2(6), b = 1349.8(6), c = 1365.5(6) pm, « = 93.55(4)°, ß = 111.23(4)°, y = 93.15(4)°. The com pound con­ sists o f SbCl6-anions, included 18-crown-6 and acetonitrile molecules, and cations [VCl(OH)(18-crown-6)(CH3C N)2]+, in which the vanadium atom is octahedrally coordinated by two nitrogen atoms o f the acetonitrile molecules in trans positions, by a chlorine atom and a hydroxyl group in cis position, and by two oxygen atom s o f the crown ether molecule. One o f the acetonitrile molecules forms weak hydrogen bridges with two oxygen atom s o f the includ­ ed crown ether molecule as well as with one chlorine atom o f the SbCl6" ion. 
  Reference    Z. Naturforsch. 48b, 149—155 (1993); eingegangen am 4. September 1992 
  Published    1993 
  Keywords    Crown Ether Complexes, Titanium, Vanadium, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/48/ZNB-1993-48b-0149.pdf 
 Identifier    ZNB-1993-48b-0149 
 Volume    48