In accordance with the procedure described by E. Wiberg, Me3Al-NH3 was heated as a bulk material in inert atmosphere to give a colorless liquid which slowly loses methane. Close to the end of this elimination reaction, the melt crystallized to give a microcrystalline powder of (Me2AlNH2)(x). The structure of this intermediate has been solved by the method of high-resolution X-ray powder diffraction. The compound crystallizes in the monoclinic space group C2/c with the cell parameters of a = 15.0047(6) Angstrom, b = 8.7500(2) Angstrom, c = 24.4702(8) Angstrom, and beta = 107.290(2)degrees, with eight trimers (Me(2)AINH(2))(3) Per unit cell. These trimers crystallize in a boat conformation in contrast to the known trimers of the same composition where a twist-boat conformation had been found by single crystal determination. Different conformers of (Me2AINH2)3 have been investigated by theoretical methods (HF/6-31G(d), B3LYP/6-31 G(d), B3LYP/6-311G(d,p), MP2(fc)/6-31 G(d), and MP2(fc)/6-311G(d,p)). The twist-boat and the chair conformer correspond to minima at the potential energy surface, whereas the boat conformer corresponds to a first-order transition state (relative energies of 0.45-2.56 kJ/mol (boat) and 6.66-11.91 kJ/mol (chair)). Relaxed scans of the potential energy surface at the HF/6-31G(d) and B3LYP/6-31G(d) levels have shown that the boat conformer (C-s symmetry) connects two enantiomers of the twist-boat form (C-2 symmetry).