KAlSb4 crystallizes in the orthorhombic Pnma space group. K(1) is bonded in a 7-coordinate geometry to two equivalent Sb(2), two equivalent Sb(3), and three equivalent Sb(1) atoms. Al(1) is bonded to one Sb(2), one Sb(3), and two equivalent Sb(1) atoms to form corner-sharing AlSb4 tetrahedra. There are four inequivalent Sb sites. In the first Sb site, Sb(1) is bonded in a 6-coordinate geometry to three equivalent K(1), two equivalent Al(1), and one Sb(4) atom. In the second Sb site, Sb(2) is bonded in a 5-coordinate geometry to two equivalent K(1), one Al(1), and two equivalent Sb(4) atoms. In the third Sb site, Sb(3) is bonded in a 5-coordinate geometry to two equivalent K(1), one Al(1), and two equivalent Sb(3) atoms. In the fourth Sb site, Sb(4) is bonded in a 3-coordinate geometry to one Sb(1) and two equivalent Sb(2) atoms.
KAlSb4 crystallizes in the orthorhombic Pnma space group. K(1) is bonded in a 7-coordinate geometry to two equivalent Sb(2), two equivalent Sb(3), and three equivalent Sb(1) atoms. Both K(1)-Sb(2) bond lengths are 3.64 Å. Both K(1)-Sb(3) bond lengths are 3.72 Å. There are two shorter (3.70 Å) and one longer (3.72 Å) K(1)-Sb(1) bond length. Al(1) is bonded to one Sb(2), one Sb(3), and two equivalent Sb(1) atoms to form corner-sharing AlSb4 tetrahedra. The Al(1)-Sb(2) bond length is 2.70 Å. The Al(1)-Sb(3) bond length is 2.71 Å. Both Al(1)-Sb(1) bond lengths are 2.69 Å. There are four inequivalent Sb sites. In the first Sb site, Sb(1) is bonded in a 6-coordinate geometry to three equivalent K(1), two equivalent Al(1), and one Sb(4) atom. The Sb(1)-Sb(4) bond length is 2.86 Å. In the second Sb site, Sb(2) is bonded in a 5-coordinate geometry to two equivalent K(1), one Al(1), and two equivalent Sb(4) atoms. Both Sb(2)-Sb(4) bond lengths are 2.88 Å. In the third Sb site, Sb(3) is bonded in a 5-coordinate geometry to two equivalent K(1), one Al(1), and two equivalent Sb(3) atoms. Both Sb(3)-Sb(3) bond lengths are 2.88 Å. In the fourth Sb site, Sb(4) is bonded in a 3-coordinate geometry to one Sb(1) and two equivalent Sb(2) atoms.