Abstract: | The Crystal Structure of Li · 11/3 H2O · C7H8]{(CH3)3Si}3C–GaI3], a Stable Hydrate of Lithium Tris(trimethylsilyl)methyl Triiodogallate Water‐free LiTsi–GaI3], prepared from gallium triiodide and base‐free Tsi–Li (Tsi = –C(SiMe3)3) in toluene, which has been recrystallized several times from humid toluene, c‐hexane, benzene and toluene again gives the water‐containing title compound. According to the X‐ray structure determination this product crystallizes in the monoclinic space group P21/c and consists of three‐membered units of Tsi–GaI3]–‐anions forming an asymmetric triangle and a related chain of three Li cations, four fold but dissimilar coordinated by the oxygen atoms of 4 water molecules, the iodligands of different anions and a h2‐bonded toluene molecule, respectively. |