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TiCl 4 (THF) 2  reacts with two equivalents of sodium in THF to afford the soluble TiCl 2 (THF)n (1), which has been characterized analytically and by spectroscopic and magnetic measurements. By redox reactions. TiCl 2 (THF) n  gives TiCl 2 (9,10-C 10 H 8 O 2 ) (2), or TiCl 2 (benzoate) 2  .(3), with 9,10-phenanthrenequinone or dibenzoylperoxide in toluene, respectively. By operating in 1,2-dimethoxyethane (DME), Na(DME) 1.5 [TiCl 4 (DME)] (4), or NaTiCl 3 (DME) 2  have been isolated from the reaction of TiCl 4 (DME) with one or two equivalents of sodium, respectively. From 4, by cation exchange, PPN[TiCl 4 (DME)] [PPN = bis(triphenylphosphine)iminium] (5), has been obtained and characterized analytically, spectroscopically and by X-ray diffraction methods. Crystal data: C 40 HCl 4 NO 2 P 2 Ti. MW = 818.4, space group: Pna2 1  (N° 33). a = 14.445(2), b = 15.690(2), c = 17.544(2) Å . V = 3976(2) Å 3 , Z = 4, F(000) = 1692, R = 0.041, Rw = 0.0420. The titanium(III) atom in the anion has the expected cis-octahedral, slightly distorted, geometry. By reaction of TiBr 4 (DME) 0.5  with sodium in DME, TiBr 3 (DME) 1.5  .1.5 DM E (7), is the product. Bis(mesitylene)vanadium(0), Vmes 2 , reacts with two equivalents of CPh 3 Cl in DME, to give VCl 2 (DME) n .

zeitschrift für naturforschung b

New Preparative Methods for the Halides of Titanium(II) and Vanadium(II): Reduction of Titanium(IV) Halides with Sodium and Oxidation of Bis(mesitylene)vanadium(0)