METALLOCENE CHEMISTRY OF HIGHLY FLUORIDATED LIGAND SYSTEMS .11. SYNTHESIS AND CHARACTERIZATION OF CP2TI(SBF6)2 AND CP2TI(SB2F11)2 - STRUCTURE OF CP2TI(SBF6)2 AND CP2V(SBF6)2

The reaction of Cp2TiF2 with two equivalents of SbF5 in liquid sulfur dioxide affords Cp2Ti(SbF6)2 in quantitative yield. The equilibrium in SO2 solution of Cp2Ti(SbF6)2 with SbF5 is completely shifted to Cp2(Ti(Sb2F11)2, which however, gives off SbF5 by crystallization to give the highly crystalline Cp2Ti(SbF6)2. The isostructural Cp2V(SbF6)2 was prepared from Cp2VCl2 and AgSbF6 in SO2 and recrystallized from a mixture of SO2/SO2ClF. The structures of Cp2Ti(SbF6)2 and Cp2V(SbF6)2 have been determined by single crystal X-ray diffraction studies. © 1990.