Yb3Sm3S8 crystallizes in the monoclinic C2 space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 8-coordinate geometry to two equivalent S(1), two equivalent S(2), two equivalent S(3), and two equivalent S(4) atoms. In the second Yb site, Yb(2) is bonded to two equivalent S(1), two equivalent S(2), two equivalent S(3), and two equivalent S(4) atoms to form distorted YbS8 hexagonal bipyramids that share corners with four equivalent Sm(2)S8 hexagonal bipyramids, edges with four equivalent Sm(1)S8 hexagonal bipyramids, and faces with four equivalent Sm(2)S8 hexagonal bipyramids. There are two inequivalent Sm sites. In the first Sm site, Sm(1) is bonded to two equivalent S(1), two equivalent S(2), two equivalent S(3), and two equivalent S(4) atoms to form distorted SmS8 hexagonal bipyramids that share corners with four equivalent Sm(2)S8 hexagonal bipyramids, edges with four equivalent Yb(2)S8 hexagonal bipyramids, and faces with four equivalent Sm(2)S8 hexagonal bipyramids. In the second Sm site, Sm(2) is bonded to two equivalent S(1), two equivalent S(2), two equivalent S(3), and two equivalent S(4) atoms to form distorted SmS8 hexagonal bipyramids that share corners with two equivalent Yb(2)S8 hexagonal bipyramids, corners with two equivalent Sm(1)S8 hexagonal bipyramids, edges with four equivalent Sm(2)S8 hexagonal bipyramids, faces with two equivalent Yb(2)S8 hexagonal bipyramids, and faces with two equivalent Sm(1)S8 hexagonal bipyramids. There are four inequivalent S sites. In the first S site, S(1) is bonded to one Yb(2), two equivalent Yb(1), one Sm(1), and two equivalent Sm(2) atoms to form a mixture of distorted edge, corner, and face-sharing SYb3Sm3 octahedra. The corner-sharing octahedral tilt angles range from 17-50°. In the second S site, S(2) is bonded to one Yb(2), two equivalent Yb(1), one Sm(1), and two equivalent Sm(2) atoms to form a mixture of distorted edge, corner, and face-sharing SYb3Sm3 octahedra. The corner-sharing octahedral tilt angles range from 17-50°. In the third S site, S(3) is bonded to one Yb(2), two equivalent Yb(1), one Sm(1), and two equivalent Sm(2) atoms to form a mixture of distorted edge, corner, and face-sharing SYb3Sm3 octahedra. The corner-sharing octahedral tilt angles range from 16-50°. In the fourth S site, S(4) is bonded to one Yb(2), two equivalent Yb(1), one Sm(1), and two equivalent Sm(2) atoms to form a mixture of distorted edge, corner, and face-sharing SYb3Sm3 octahedra. The corner-sharing octahedral tilt angles range from 17-50°.
Yb3Sm3S8 crystallizes in the monoclinic C2 space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 8-coordinate geometry to two equivalent S(1), two equivalent S(2), two equivalent S(3), and two equivalent S(4) atoms. There is one shorter (2.83 Å) and one longer (3.08 Å) Yb(1)-S(1) bond length. There is one shorter (2.81 Å) and one longer (3.05 Å) Yb(1)-S(2) bond length. There is one shorter (2.82 Å) and one longer (3.07 Å) Yb(1)-S(3) bond length. There is one shorter (2.83 Å) and one longer (3.06 Å) Yb(1)-S(4) bond length. In the second Yb site, Yb(2) is bonded to two equivalent S(1), two equivalent S(2), two equivalent S(3), and two equivalent S(4) atoms to form distorted YbS8 hexagonal bipyramids that share corners with four equivalent Sm(2)S8 hexagonal bipyramids, edges with four equivalent Sm(1)S8 hexagonal bipyramids, and faces with four equivalent Sm(2)S8 hexagonal bipyramids. Both Yb(2)-S(1) bond lengths are 3.04 Å. Both Yb(2)-S(2) bond lengths are 3.04 Å. Both Yb(2)-S(3) bond lengths are 2.82 Å. Both Yb(2)-S(4) bond lengths are 2.84 Å. There are two inequivalent Sm sites. In the first Sm site, Sm(1) is bonded to two equivalent S(1), two equivalent S(2), two equivalent S(3), and two equivalent S(4) atoms to form distorted SmS8 hexagonal bipyramids that share corners with four equivalent Sm(2)S8 hexagonal bipyramids, edges with four equivalent Yb(2)S8 hexagonal bipyramids, and faces with four equivalent Sm(2)S8 hexagonal bipyramids. Both Sm(1)-S(1) bond lengths are 2.82 Å. Both Sm(1)-S(2) bond lengths are 2.82 Å. Both Sm(1)-S(3) bond lengths are 3.00 Å. Both Sm(1)-S(4) bond lengths are 3.00 Å. In the second Sm site, Sm(2) is bonded to two equivalent S(1), two equivalent S(2), two equivalent S(3), and two equivalent S(4) atoms to form distorted SmS8 hexagonal bipyramids that share corners with two equivalent Yb(2)S8 hexagonal bipyramids, corners with two equivalent Sm(1)S8 hexagonal bipyramids, edges with four equivalent Sm(2)S8 hexagonal bipyramids, faces with two equivalent Yb(2)S8 hexagonal bipyramids, and faces with two equivalent Sm(1)S8 hexagonal bipyramids. There is one shorter (2.83 Å) and one longer (2.98 Å) Sm(2)-S(1) bond length. There is one shorter (2.84 Å) and one longer (3.00 Å) Sm(2)-S(2) bond length. There is one shorter (2.84 Å) and one longer (2.99 Å) Sm(2)-S(3) bond length. There is one shorter (2.83 Å) and one longer (3.00 Å) Sm(2)-S(4) bond length. There are four inequivalent S sites. In the first S site, S(1) is bonded to one Yb(2), two equivalent Yb(1), one Sm(1), and two equivalent Sm(2) atoms to form a mixture of distorted edge, corner, and face-sharing SYb3Sm3 octahedra. The corner-sharing octahedral tilt angles range from 17-50°. In the second S site, S(2) is bonded to one Yb(2), two equivalent Yb(1), one Sm(1), and two equivalent Sm(2) atoms to form a mixture of distorted edge, corner, and face-sharing SYb3Sm3 octahedra. The corner-sharing octahedral tilt angles range from 17-50°. In the third S site, S(3) is bonded to one Yb(2), two equivalent Yb(1), one Sm(1), and two equivalent Sm(2) atoms to form a mixture of distorted edge, corner, and face-sharing SYb3Sm3 octahedra. The corner-sharing octahedral tilt angles range from 16-50°. In the fourth S site, S(4) is bonded to one Yb(2), two equivalent Yb(1), one Sm(1), and two equivalent Sm(2) atoms to form a mixture of distorted edge, corner, and face-sharing SYb3Sm3 octahedra. The corner-sharing octahedral tilt angles range from 17-50°.