Abstract The crystal structure of tribenzylaluminum· diethyl etherate has been determined by single crystal X-ray diffraction techniques. It crystallizes in the monoclinic system, space group P2 1, with unit cell dimensions of a 8.106 (1), b 15.098 (2), c 10.037 (1) Å, β 111.02 (1), V 1146.6 (3) Å 3, and Z= 2. The final full matrix least-squares refinement on 1139 data gave RF 3.8 and R wF 5.2%. The compound is similar to other organoaluminum adducts ...