Fe2BiSbO7 crystallizes in the orthorhombic Imma space group. There are two inequivalent Fe sites. In the first Fe site, Fe(1) is bonded in a 8-coordinate geometry to two equivalent O(1), two equivalent O(4), and four equivalent O(3) atoms. In the second Fe site, Fe(2) is bonded in a body-centered cubic geometry to two equivalent O(2), two equivalent O(4), and four equivalent O(3) atoms. Bi(1) is bonded to two equivalent O(2) and four equivalent O(3) atoms to form BiO6 octahedra that share corners with two equivalent Bi(1)O6 octahedra and corners with four equivalent Sb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 52-59°. Sb(1) is bonded to two equivalent O(1) and four equivalent O(3) atoms to form SbO6 octahedra that share corners with two equivalent Sb(1)O6 octahedra and corners with four equivalent Bi(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 39-52°. There are four inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 150 degrees geometry to two equivalent Fe(1) and two equivalent Sb(1) atoms. In the second O site, O(2) is bonded to two equivalent Fe(2) and two equivalent Bi(1) atoms to form OFe2Bi2 tetrahedra that share corners with two equivalent O(4)Fe4 tetrahedra, corners with four equivalent O(2)Fe2Bi2 tetrahedra, and  an edgeedge with one O(4)Fe4 tetrahedra. In the third O site, O(3) is bonded in a 4-coordinate geometry to one Fe(1), one Fe(2), one Bi(1), and one Sb(1) atom. In the fourth O site, O(4) is bonded to two equivalent Fe(1) and two equivalent Fe(2) atoms to form OFe4 tetrahedra that share corners with two equivalent O(2)Fe2Bi2 tetrahedra, corners with four equivalent O(4)Fe4 tetrahedra, and  an edgeedge with one O(2)Fe2Bi2 tetrahedra.
Fe2BiSbO7 crystallizes in the orthorhombic Imma space group. There are two inequivalent Fe sites. In the first Fe site, Fe(1) is bonded in a 8-coordinate geometry to two equivalent O(1), two equivalent O(4), and four equivalent O(3) atoms. Both Fe(1)-O(1) bond lengths are 2.70 Å. Both Fe(1)-O(4) bond lengths are 2.22 Å. All Fe(1)-O(3) bond lengths are 2.42 Å. In the second Fe site, Fe(2) is bonded in a body-centered cubic geometry to two equivalent O(2), two equivalent O(4), and four equivalent O(3) atoms. Both Fe(2)-O(2) bond lengths are 2.39 Å. Both Fe(2)-O(4) bond lengths are 2.30 Å. All Fe(2)-O(3) bond lengths are 2.62 Å. Bi(1) is bonded to two equivalent O(2) and four equivalent O(3) atoms to form BiO6 octahedra that share corners with two equivalent Bi(1)O6 octahedra and corners with four equivalent Sb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 52-59°. Both Bi(1)-O(2) bond lengths are 2.15 Å. All Bi(1)-O(3) bond lengths are 2.12 Å. Sb(1) is bonded to two equivalent O(1) and four equivalent O(3) atoms to form SbO6 octahedra that share corners with two equivalent Sb(1)O6 octahedra and corners with four equivalent Bi(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 39-52°. Both Sb(1)-O(1) bond lengths are 1.94 Å. All Sb(1)-O(3) bond lengths are 1.99 Å. There are four inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 150 degrees geometry to two equivalent Fe(1) and two equivalent Sb(1) atoms. In the second O site, O(2) is bonded to two equivalent Fe(2) and two equivalent Bi(1) atoms to form OFe2Bi2 tetrahedra that share corners with two equivalent O(4)Fe4 tetrahedra, corners with four equivalent O(2)Fe2Bi2 tetrahedra, and  an edgeedge with one O(4)Fe4 tetrahedra. In the third O site, O(3) is bonded in a 4-coordinate geometry to one Fe(1), one Fe(2), one Bi(1), and one Sb(1) atom. In the fourth O site, O(4) is bonded to two equivalent Fe(1) and two equivalent Fe(2) atoms to form OFe4 tetrahedra that share corners with two equivalent O(2)Fe2Bi2 tetrahedra, corners with four equivalent O(4)Fe4 tetrahedra, and  an edgeedge with one O(2)Fe2Bi2 tetrahedra.