CaSb2O4 is Spinel-like structured and crystallizes in the orthorhombic Imma space group. Ca(1) is bonded to two equivalent O(2) and four equivalent O(1) atoms to form CaO6 octahedra that share corners with six equivalent Sb(1)O4 tetrahedra, edges with two equivalent Ca(1)O6 octahedra, and edges with four equivalent Sb(2)O6 octahedra. There are two inequivalent Sb sites. In the first Sb site, Sb(1) is bonded to two equivalent O(1) and two equivalent O(2) atoms to form SbO4 tetrahedra that share corners with six equivalent Ca(1)O6 octahedra and corners with six equivalent Sb(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 50-70°. In the second Sb site, Sb(2) is bonded to two equivalent O(1) and four equivalent O(2) atoms to form SbO6 octahedra that share corners with six equivalent Sb(1)O4 tetrahedra, edges with two equivalent Sb(2)O6 octahedra, and edges with four equivalent Ca(1)O6 octahedra. There are two inequivalent O sites. In the first O site, O(1) is bonded in a rectangular see-saw-like geometry to two equivalent Ca(1), one Sb(1), and one Sb(2) atom. In the second O site, O(2) is bonded in a rectangular see-saw-like geometry to one Ca(1), one Sb(1), and two equivalent Sb(2) atoms.
CaSb2O4 is Spinel-like structured and crystallizes in the orthorhombic Imma space group. Ca(1) is bonded to two equivalent O(2) and four equivalent O(1) atoms to form CaO6 octahedra that share corners with six equivalent Sb(1)O4 tetrahedra, edges with two equivalent Ca(1)O6 octahedra, and edges with four equivalent Sb(2)O6 octahedra. Both Ca(1)-O(2) bond lengths are 2.35 Å. All Ca(1)-O(1) bond lengths are 2.48 Å. There are two inequivalent Sb sites. In the first Sb site, Sb(1) is bonded to two equivalent O(1) and two equivalent O(2) atoms to form SbO4 tetrahedra that share corners with six equivalent Ca(1)O6 octahedra and corners with six equivalent Sb(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 50-70°. Both Sb(1)-O(1) bond lengths are 2.08 Å. Both Sb(1)-O(2) bond lengths are 2.32 Å. In the second Sb site, Sb(2) is bonded to two equivalent O(1) and four equivalent O(2) atoms to form SbO6 octahedra that share corners with six equivalent Sb(1)O4 tetrahedra, edges with two equivalent Sb(2)O6 octahedra, and edges with four equivalent Ca(1)O6 octahedra. Both Sb(2)-O(1) bond lengths are 2.36 Å. All Sb(2)-O(2) bond lengths are 2.30 Å. There are two inequivalent O sites. In the first O site, O(1) is bonded in a rectangular see-saw-like geometry to two equivalent Ca(1), one Sb(1), and one Sb(2) atom. In the second O site, O(2) is bonded in a rectangular see-saw-like geometry to one Ca(1), one Sb(1), and two equivalent Sb(2) atoms.