The Crystal Structure of γ‐AlD3.

Abstract γ-AlD 3 was synthesized from LiAlD 4 and AlCl 3 via thermal decomposition of aluminum hydride etherate in presence of excess LiAlD 4 . γ-AlD 3 was determined by powder neutron diffraction and synchrotron X-ray diffraction to crystallize in the space group Pnnm . The orthorhombic structure has unit-cell dimensions a  = 7.3360(3) A, b  = 5.3672(2) A and c  = 5.7562(1) A, and it consists of both corner- and edge-sharing AlD 6 octahedra where each hydrogen is shared between two octahedra. The average Al–D distances in octahedra with edge-sharing is 1.706 A and in the octahedra with only corner-sharing 1.719 A.