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By the reaction of (Me 3 SiNH) 2 SiClNMe 2  with TiCl 4  the by-product [Me 2 NH 2 ] 2 [TiCl 6 ] was obtained in form of crystals suitable for single-crystal XRD (Pnnm, Z = 2, a = 722.01(3), b = 1428.36(5), c = 703.31(3) pm, T = 200 K, 901 independent reflections, 57 variables, R1 = 0.0636). The product was also synthesized in higher yield by the stoichiometric reaction of two equivalents of [Me 2 NH 2 ]Cl with TiCl 4  in CHCl 3  at room temperature as a yellow crystalline powder. Bis(dimethylammonium) hexachlorotitanate is built up from [TiCl 6 ] 2-  anions forming elongated octahedra and [Me 2 NH 2 ] +  ions. The [TiCl 6 ] 2-  ions are connected by the [Me 2 NH 2 ] +  ions through N-H···Cl hydrogen bridges forming an arrangement which resembles that of an expanded rutile structure type. The elongation of the [TiCl 6 ]2 -  octahedra was also verified by IR and Raman spectroscopy, confirming a local symmetry reduction from O h  to D 4h . The solubility of [Me 2 NH 2 ] 2 [TiCl 6 ] in MeNO 2  and MeCN was determined by means of  14 N-NMR to be about 0.1 mol% and 0.3 mol%, respectively.

zeitschrift für naturforschung b

Synthese, Kristallstruktur und spektroskopische Charakterisierung von Bis(dimethylammonium)hexachlorotitanat [Me 2 NH 2 ] 2 [TiCl 6 ]/ Synthesis, Crystal Structure, and Spectroscopic Characterization of Bis(dimethylammonium) Hexachlorotitanate [Me 2 NH 2 ] 2 [TiCl 6 ]