Cationic Titanium(IV) Complexes via Halide Abstraction from : Crystal and Molecular Structure of 3*2MeCN

Article abstract of DOI:10.1039/DT9940000305

Treatment of (cp=η⁵-C5H5) with SbCl5 as chloride abstractor in acetonitrile provided hexachloroantimonate(V) salts of (1+), (2+) and (3+) respectively.With 1:1 stoichiometry red-brown crystals of 1 are obtained and with 1:2 stoichiometry light blue crystals of 2 2.Complete removal of chloride ion from requires a six-fold excess of SbCl5 when purple-blue crystals of 3 3 can be isolated.These products were characterised by analytical and spectroscopic (IR, 1H NMR) data and, in the case of 3, by a crystal structure determination.Proton NMR studies indicate the presence of intermediate halide-bridged species in solution during the sequential halide abstractions 1 --> 2 --> 3.Crystals of complex 3, obtained as the bis(solvate) from recrystallisation in acetonitrile, are monoclinic and X-ray structural analysis confirmed the formulation.The crystal structure a=19.650(4), b=19.182(4), c=12.958(3) Angstroem, β=91.612(3) deg, Z=4, R=0.0386, R'=0.0406> shows discrete cations and anions and a pseudo-octahedral co-ordination sphere for the Ti(IV).A significant trans influence of the cyclopentadienyl ligand affects Ti-N bond lengths in the complex.

Full text of DOI:10.1039/DT9940000305

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