Ni3GaSb crystallizes in the hexagonal P-6m2 space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a 11-coordinate geometry to two equivalent Ni(1), three equivalent Ni(2), three equivalent Ga(1), and three equivalent Sb(1) atoms. In the second Ni site, Ni(2) is bonded to six equivalent Ni(1), two equivalent Ga(1), and three equivalent Sb(1) atoms to form a mixture of distorted face and corner-sharing NiGa2Ni6Sb3 trigonal bipyramids. Ga(1) is bonded in a 8-coordinate geometry to two equivalent Ni(2) and six equivalent Ni(1) atoms. Sb(1) is bonded in a 9-coordinate geometry to three equivalent Ni(2) and six equivalent Ni(1) atoms.
Ni3GaSb crystallizes in the hexagonal P-6m2 space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a 11-coordinate geometry to two equivalent Ni(1), three equivalent Ni(2), three equivalent Ga(1), and three equivalent Sb(1) atoms. There is one shorter (2.44 Å) and one longer (2.53 Å) Ni(1)-Ni(1) bond length. All Ni(1)-Ni(2) bond lengths are 2.70 Å. All Ni(1)-Ga(1) bond lengths are 2.68 Å. All Ni(1)-Sb(1) bond lengths are 2.70 Å. In the second Ni site, Ni(2) is bonded to six equivalent Ni(1), two equivalent Ga(1), and three equivalent Sb(1) atoms to form a mixture of distorted face and corner-sharing NiGa2Ni6Sb3 trigonal bipyramids. Both Ni(2)-Ga(1) bond lengths are 2.48 Å. All Ni(2)-Sb(1) bond lengths are 2.38 Å. Ga(1) is bonded in a 8-coordinate geometry to two equivalent Ni(2) and six equivalent Ni(1) atoms. Sb(1) is bonded in a 9-coordinate geometry to three equivalent Ni(2) and six equivalent Ni(1) atoms.