Yb2FeSbO7 crystallizes in the orthorhombic Imma space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to two equivalent O(2), two equivalent O(4), and four equivalent O(3) atoms to form distorted YbO8 hexagonal bipyramids that share edges with two equivalent Yb(1)O8 hexagonal bipyramids, edges with four equivalent Yb(2)O8 hexagonal bipyramids, edges with two equivalent Fe(1)O6 octahedra, and edges with four equivalent Sb(1)O6 octahedra. In the second Yb site, Yb(2) is bonded to two equivalent O(1), two equivalent O(4), and four equivalent O(3) atoms to form distorted YbO8 hexagonal bipyramids that share edges with two equivalent Yb(2)O8 hexagonal bipyramids, edges with four equivalent Yb(1)O8 hexagonal bipyramids, edges with two equivalent Sb(1)O6 octahedra, and edges with four equivalent Fe(1)O6 octahedra. Fe(1) is bonded to two equivalent O(1) and four equivalent O(3) atoms to form FeO6 octahedra that share corners with two equivalent Fe(1)O6 octahedra, corners with four equivalent Sb(1)O6 octahedra, edges with two equivalent Yb(1)O8 hexagonal bipyramids, and edges with four equivalent Yb(2)O8 hexagonal bipyramids. The corner-sharing octahedral tilt angles range from 43-48°. Sb(1) is bonded to two equivalent O(2) and four equivalent O(3) atoms to form SbO6 octahedra that share corners with two equivalent Sb(1)O6 octahedra, corners with four equivalent Fe(1)O6 octahedra, edges with two equivalent Yb(2)O8 hexagonal bipyramids, and edges with four equivalent Yb(1)O8 hexagonal bipyramids. The corner-sharing octahedral tilt angles range from 48-50°. There are four inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to two equivalent Yb(2) and two equivalent Fe(1) atoms. In the second O site, O(2) is bonded to two equivalent Yb(1) and two equivalent Sb(1) atoms to form distorted OYb2Sb2 tetrahedra that share corners with two equivalent O(4)Yb4 tetrahedra, corners with four equivalent O(2)Yb2Sb2 tetrahedra, corners with eight equivalent O(3)Yb2FeSb tetrahedra,  an edgeedge with one O(4)Yb4 tetrahedra, and edges with four equivalent O(3)Yb2FeSb tetrahedra. In the third O site, O(3) is bonded to one Yb(1), one Yb(2), one Fe(1), and one Sb(1) atom to form distorted OYb2FeSb tetrahedra that share corners with two equivalent O(2)Yb2Sb2 tetrahedra, corners with two equivalent O(4)Yb4 tetrahedra, corners with eight equivalent O(3)Yb2FeSb tetrahedra,  an edgeedge with one O(2)Yb2Sb2 tetrahedra,  an edgeedge with one O(4)Yb4 tetrahedra, and edges with two equivalent O(3)Yb2FeSb tetrahedra. In the fourth O site, O(4) is bonded to two equivalent Yb(1) and two equivalent Yb(2) atoms to form OYb4 tetrahedra that share corners with two equivalent O(2)Yb2Sb2 tetrahedra, corners with four equivalent O(4)Yb4 tetrahedra, corners with eight equivalent O(3)Yb2FeSb tetrahedra,  an edgeedge with one O(2)Yb2Sb2 tetrahedra, and edges with four equivalent O(3)Yb2FeSb tetrahedra.
Yb2FeSbO7 crystallizes in the orthorhombic Imma space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to two equivalent O(2), two equivalent O(4), and four equivalent O(3) atoms to form distorted YbO8 hexagonal bipyramids that share edges with two equivalent Yb(1)O8 hexagonal bipyramids, edges with four equivalent Yb(2)O8 hexagonal bipyramids, edges with two equivalent Fe(1)O6 octahedra, and edges with four equivalent Sb(1)O6 octahedra. Both Yb(1)-O(2) bond lengths are 2.47 Å. Both Yb(1)-O(4) bond lengths are 2.22 Å. All Yb(1)-O(3) bond lengths are 2.55 Å. In the second Yb site, Yb(2) is bonded to two equivalent O(1), two equivalent O(4), and four equivalent O(3) atoms to form distorted YbO8 hexagonal bipyramids that share edges with two equivalent Yb(2)O8 hexagonal bipyramids, edges with four equivalent Yb(1)O8 hexagonal bipyramids, edges with two equivalent Sb(1)O6 octahedra, and edges with four equivalent Fe(1)O6 octahedra. Both Yb(2)-O(1) bond lengths are 2.59 Å. Both Yb(2)-O(4) bond lengths are 2.21 Å. All Yb(2)-O(3) bond lengths are 2.49 Å. Fe(1) is bonded to two equivalent O(1) and four equivalent O(3) atoms to form FeO6 octahedra that share corners with two equivalent Fe(1)O6 octahedra, corners with four equivalent Sb(1)O6 octahedra, edges with two equivalent Yb(1)O8 hexagonal bipyramids, and edges with four equivalent Yb(2)O8 hexagonal bipyramids. The corner-sharing octahedral tilt angles range from 43-48°. Both Fe(1)-O(1) bond lengths are 1.94 Å. All Fe(1)-O(3) bond lengths are 1.96 Å. Sb(1) is bonded to two equivalent O(2) and four equivalent O(3) atoms to form SbO6 octahedra that share corners with two equivalent Sb(1)O6 octahedra, corners with four equivalent Fe(1)O6 octahedra, edges with two equivalent Yb(2)O8 hexagonal bipyramids, and edges with four equivalent Yb(1)O8 hexagonal bipyramids. The corner-sharing octahedral tilt angles range from 48-50°. Both Sb(1)-O(2) bond lengths are 2.01 Å. All Sb(1)-O(3) bond lengths are 2.00 Å. There are four inequivalent O sites. In the first O site, O(1) is bonded in a 4-coordinate geometry to two equivalent Yb(2) and two equivalent Fe(1) atoms. In the second O site, O(2) is bonded to two equivalent Yb(1) and two equivalent Sb(1) atoms to form distorted OYb2Sb2 tetrahedra that share corners with two equivalent O(4)Yb4 tetrahedra, corners with four equivalent O(2)Yb2Sb2 tetrahedra, corners with eight equivalent O(3)Yb2FeSb tetrahedra,  an edgeedge with one O(4)Yb4 tetrahedra, and edges with four equivalent O(3)Yb2FeSb tetrahedra. In the third O site, O(3) is bonded to one Yb(1), one Yb(2), one Fe(1), and one Sb(1) atom to form distorted OYb2FeSb tetrahedra that share corners with two equivalent O(2)Yb2Sb2 tetrahedra, corners with two equivalent O(4)Yb4 tetrahedra, corners with eight equivalent O(3)Yb2FeSb tetrahedra,  an edgeedge with one O(2)Yb2Sb2 tetrahedra,  an edgeedge with one O(4)Yb4 tetrahedra, and edges with two equivalent O(3)Yb2FeSb tetrahedra. In the fourth O site, O(4) is bonded to two equivalent Yb(1) and two equivalent Yb(2) atoms to form OYb4 tetrahedra that share corners with two equivalent O(2)Yb2Sb2 tetrahedra, corners with four equivalent O(4)Yb4 tetrahedra, corners with eight equivalent O(3)Yb2FeSb tetrahedra,  an edgeedge with one O(2)Yb2Sb2 tetrahedra, and edges with four equivalent O(3)Yb2FeSb tetrahedra.