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CROWN-ETHER COMPLEXATION OF TITANIUM - SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF A CATIONIC OXYGEN-BRIDGED TITANIUM(IV) DIMER

Publisher
ROYAL SOC CHEMISTRY
Publication Date
Keywords
  • Qd Chemistry

Abstract

1,4,7,10-Tetraoxacyclododecane (12-crown-4) reacts with [TiCl3(MeCN)3] [SbCl6] in MeCN to form a complex which provides the crown ether titanoxane [{TiCl(mu-O)(12-crown-4)}2] [SbCl6]2.2CH2Cl2 1 following inadvertent hydrolysis. The structure of 1 contains a discrete di-mu-oxo-dititanium cation placed on a crystallographic centre of inversion, two regular (O(h)) SbCl6- anions and two molecules of CH2Cl2 as lattice solvate. The complex crystallises in the space group P2(1)/n with cell dimensions a = 8.337(4), b = 21.307(10), c = 13.626(8) angstrom, bet = 107.13(4)-degrees, with Z = 2; R = 0.038 for 3271 observed reflections [I/sigma(I) greater-than-or-equal-to 2.0]. The core Ti2O2 ring is planar with dimensions Ti-O 1.823(4) and 1.811(3) angstrom and O-Ti-O 79.7(2) and Ti-O-Ti 100.3(2)-degrees. In addition to the two bridging oxygen atoms each titanium atom is bonded to one chlorine [Ti-Cl 2.277(2) angstrom] and all four oxygen atoms of a crown macrocycle [Ti-O 2.121(4)-2.237(4), mean 2.242 angstrom].

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