Synthesis, Spectroscopic Properties, and Crystal Structure of the Oxonium Acid [H(OEt2)2]+[Ti2Cl9]–
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Stefan Rannabauer
The oxonium acid [H(OEt2)2]+[Ti2Cl9]− (1) was obtained by the reaction of TiCl4 with Et2O in n-pentane and subsequent partial hydrolysis. Suitable single crystals of 1 were obtained by sublimation at 5° C ([H(OEt2)2]+[Ti2Cl9]−, P212121 (no. 19), Z = 4, a = 1101.08(8), b = 1328.4(2), c = 1525.0(2) pm, T = 193(2) K, 4489 independent reflections, 197 parameters, R1 = 0.049). The cation is made up from two independent Et2O molecules and one disordered proton on two split positions. Both ether molecules exhibit a W form, and their molecular planes include an angle of 74.1(7)°. Thus a distorted tetrahedron is formed by the four methyl carbon atoms of the two ether molecules. The distance O···O amounts to 237.7(1) pm. The proton of the cation was characterized both by 1H NMR (CDCl3, T = 23 °C: δ = 11.7 ppm, w1/2 = 100 Hz) and IR spectroscopy (3120 cm−1, ν vbr). The [Ti2Cl9]− ion consists of two face sharing octahedra. 47Ti and 49Ti NMR spectra were recorded in solution (CH2Cl2, T = 23 °C: δ 49Ti = 137 ppm, w1/2 = 175 Hz; δ 47Ti = −124 ppm, w1/2 = 250 Hz). The absence of a signal for TiCl4 at δ 49Ti = 0 ppm indicates the stability of the dinuclear anion in solution.
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Articles in the same Issue
- Triiodotelluronium Hexafluoroarsenate TeI3[AsF6]. The Crystal Structure of the Hemi SO2 Solvate and the Structure Relation to the Unsolvated Form
- peri-Interactions in Naphthalenes, 11 . A New Approach to the Investigation of Dative peri Bonding/A New Approach to the Investigation of Dative peri Bonding
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- Synthesis and Structure of YbIrIn5
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