CsDy2Cu3S5 crystallizes in the orthorhombic Cmcm space group. Cs(1) is bonded in a 10-coordinate geometry to two equivalent Cu(1), two equivalent S(1), two equivalent S(3), and four equivalent S(2) atoms. Dy(1) is bonded to one S(1), two equivalent S(2), and three equivalent S(3) atoms to form DyS6 octahedra that share  a cornercorner with one Dy(1)S6 octahedra, corners with four equivalent Cu(2)S4 tetrahedra, edges with four equivalent Dy(1)S6 octahedra, and edges with three equivalent Cu(2)S4 tetrahedra. The corner-sharing octahedral tilt angles are 22°. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a 4-coordinate geometry to two equivalent Cs(1), two equivalent S(1), and two equivalent S(2) atoms. In the second Cu site, Cu(2) is bonded to two equivalent S(2) and two equivalent S(3) atoms to form CuS4 tetrahedra that share corners with four equivalent Dy(1)S6 octahedra, corners with two equivalent Cu(2)S4 tetrahedra, edges with three equivalent Dy(1)S6 octahedra, and  an edgeedge with one Cu(2)S4 tetrahedra. The corner-sharing octahedral tilt angles range from 14-58°. There are three inequivalent S sites. In the first S site, S(1) is bonded in a 6-coordinate geometry to two equivalent Cs(1), two equivalent Dy(1), and two equivalent Cu(1) atoms. In the second S site, S(2) is bonded in a 7-coordinate geometry to two equivalent Cs(1), two equivalent Dy(1), one Cu(1), and two equivalent Cu(2) atoms. In the third S site, S(3) is bonded to one Cs(1), three equivalent Dy(1), and two equivalent Cu(2) atoms to form a mixture of distorted corner and edge-sharing SCsDy3Cu2 octahedra. The corner-sharing octahedral tilt angles are 52°.
CsDy2Cu3S5 crystallizes in the orthorhombic Cmcm space group. Cs(1) is bonded in a 10-coordinate geometry to two equivalent Cu(1), two equivalent S(1), two equivalent S(3), and four equivalent S(2) atoms. Both Cs(1)-Cu(1) bond lengths are 3.71 Å. Both Cs(1)-S(1) bond lengths are 3.52 Å. Both Cs(1)-S(3) bond lengths are 3.40 Å. All Cs(1)-S(2) bond lengths are 3.60 Å. Dy(1) is bonded to one S(1), two equivalent S(2), and three equivalent S(3) atoms to form DyS6 octahedra that share  a cornercorner with one Dy(1)S6 octahedra, corners with four equivalent Cu(2)S4 tetrahedra, edges with four equivalent Dy(1)S6 octahedra, and edges with three equivalent Cu(2)S4 tetrahedra. The corner-sharing octahedral tilt angles are 22°. The Dy(1)-S(1) bond length is 2.74 Å. Both Dy(1)-S(2) bond lengths are 2.72 Å. There is one shorter (2.71 Å) and two longer (2.81 Å) Dy(1)-S(3) bond lengths. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a 4-coordinate geometry to two equivalent Cs(1), two equivalent S(1), and two equivalent S(2) atoms. Both Cu(1)-S(1) bond lengths are 2.23 Å. Both Cu(1)-S(2) bond lengths are 2.76 Å. In the second Cu site, Cu(2) is bonded to two equivalent S(2) and two equivalent S(3) atoms to form CuS4 tetrahedra that share corners with four equivalent Dy(1)S6 octahedra, corners with two equivalent Cu(2)S4 tetrahedra, edges with three equivalent Dy(1)S6 octahedra, and  an edgeedge with one Cu(2)S4 tetrahedra. The corner-sharing octahedral tilt angles range from 14-58°. There is one shorter (2.38 Å) and one longer (2.44 Å) Cu(2)-S(2) bond length. Both Cu(2)-S(3) bond lengths are 2.39 Å. There are three inequivalent S sites. In the first S site, S(1) is bonded in a 6-coordinate geometry to two equivalent Cs(1), two equivalent Dy(1), and two equivalent Cu(1) atoms. In the second S site, S(2) is bonded in a 7-coordinate geometry to two equivalent Cs(1), two equivalent Dy(1), one Cu(1), and two equivalent Cu(2) atoms. In the third S site, S(3) is bonded to one Cs(1), three equivalent Dy(1), and two equivalent Cu(2) atoms to form a mixture of distorted corner and edge-sharing SCsDy3Cu2 octahedra. The corner-sharing octahedral tilt angles are 52°.