In the spinel system Li,-,Ti204 the Li content was reduced by oxidative extraction by means of a solution of I, as well as Br, in CH3CN or by oxygen. The extraction is associated with a transition of Ti3+ to Ti4+: the system is L i , -Y T i~! Y T i~~Y 0 4 . Consequently, with increasing y the charge carrier concentration decreases from the starting value of 0.5 electrons/Ti ion for LiTi204. The extraction proceeds in two steps. At the beginning, the Ti20, framework remains intact and the transition to superconductivity increases with decreasing charge carrier concentration to a maximal value of 13.2K. Separated by a two-phase region for medium extraction levels for higher y values, a Li depleted material of approximate composition Lio,,Ti,04 is obtained. The crystal structure of Lio.3Ti,0, can be deduced from the original spinel lattice by a partial Ti migration from 16d to 16c and 8a sites (space group Fd3m). Consequently, the Ti,04 framework of Lio,3Ti,0, is disconnected and the material is no longer superconducting.