| Abstract: | Lithium and Cesium Alkoxometalates The aluminium alkoxide, Al(OCH2Ph)3 ( 1 ), can be obtained from a direct synthesis of Al and PhCH2OH under HgCl2 catalysis. The formation of the metalate {(Diglyme)Li}{Al(OtBu)4}] ( 2 ) from LiAlH4 and tBuOH in THF under evolution of hydrogen takes place, if the reaction product is heated under reflux with additional tBuOH in diglyme. The nucleophilic attack of F– ions leads during the treatment of CsF on a THF solution of Al(OcHex)3 after ligand redistribution to the coordination polymer {Cs(THF)2}{Cs(THF)}{Al(OcHex)4}2]n (3]n). 1 , 2 , and 3 were characterized by NMR, IR and MS techniques as well as by crystal structure analyses. According to them 1 is present as tetramer in solution and the solid state. The central structural motif of the metalate 2 is a heteronuclear and planar LiO2Al four‐membered ring with a penta‐coordinated Li+ ion. In the chainlike coordination polymer 3 ]n Cs+ ions with coordination number five and six occupy alternating positions. |
