DyVSb3 crystallizes in the orthorhombic Pbcm space group. Dy(1) is bonded in a 9-coordinate geometry to one Sb(1), four equivalent Sb(2), and four equivalent Sb(3) atoms. V(1) is bonded to two equivalent Sb(2) and four equivalent Sb(1) atoms to form a mixture of distorted face, corner, and edge-sharing VSb6 octahedra. The corner-sharing octahedral tilt angles are 46°. There are three inequivalent Sb sites. In the first Sb site, Sb(1) is bonded in a 5-coordinate geometry to one Dy(1), four equivalent V(1), and one Sb(2) atom. In the second Sb site, Sb(2) is bonded in a 7-coordinate geometry to four equivalent Dy(1), two equivalent V(1), and one Sb(1) atom. In the third Sb site, Sb(3) is bonded in a 8-coordinate geometry to four equivalent Dy(1) and four equivalent Sb(3) atoms.
DyVSb3 crystallizes in the orthorhombic Pbcm space group. Dy(1) is bonded in a 9-coordinate geometry to one Sb(1), four equivalent Sb(2), and four equivalent Sb(3) atoms. The Dy(1)-Sb(1) bond length is 3.22 Å. There are a spread of Dy(1)-Sb(2) bond distances ranging from 3.20-3.33 Å. There are two shorter (3.21 Å) and two longer (3.24 Å) Dy(1)-Sb(3) bond lengths. V(1) is bonded to two equivalent Sb(2) and four equivalent Sb(1) atoms to form a mixture of distorted face, corner, and edge-sharing VSb6 octahedra. The corner-sharing octahedral tilt angles are 46°. Both V(1)-Sb(2) bond lengths are 2.76 Å. There are two shorter (2.73 Å) and two longer (2.76 Å) V(1)-Sb(1) bond lengths. There are three inequivalent Sb sites. In the first Sb site, Sb(1) is bonded in a 5-coordinate geometry to one Dy(1), four equivalent V(1), and one Sb(2) atom. The Sb(1)-Sb(2) bond length is 3.13 Å. In the second Sb site, Sb(2) is bonded in a 7-coordinate geometry to four equivalent Dy(1), two equivalent V(1), and one Sb(1) atom. In the third Sb site, Sb(3) is bonded in a 8-coordinate geometry to four equivalent Dy(1) and four equivalent Sb(3) atoms. There are two shorter (3.08 Å) and two longer (3.09 Å) Sb(3)-Sb(3) bond lengths.