Yb16S29 crystallizes in the triclinic P1 space group. There are sixteen inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to one S(16), one S(18), one S(22), one S(26), one S(4), and one S(8) atom to form a mixture of distorted corner, edge, and face-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles are 1°. In the second Yb site, Yb(2) is bonded in a 7-coordinate geometry to one S(10), one S(11), one S(28), one S(4), one S(5), one S(8), and one S(9) atom. In the third Yb site, Yb(3) is bonded to one S(14), one S(2), one S(22), one S(27), one S(8), and one S(9) atom to form a mixture of distorted corner and edge-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles range from 1-14°. In the fourth Yb site, Yb(4) is bonded in a 6-coordinate geometry to one S(11), one S(14), one S(16), one S(2), one S(25), one S(29), and one S(8) atom. In the fifth Yb site, Yb(5) is bonded to one S(10), one S(11), one S(14), one S(17), one S(19), and one S(9) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(10)S6 octahedra, corners with two equivalent Yb(16)S7 square pyramids,  an edgeedge with one Yb(3)S6 octahedra,  an edgeedge with one Yb(6)S6 octahedra,  an edgeedge with one Yb(7)S6 octahedra,  an edgeedge with one Yb(8)S6 octahedra, and  an edgeedge with one Yb(9)S6 octahedra. The corner-sharing octahedral tilt angles range from 1-3°. In the sixth Yb site, Yb(6) is bonded to one S(11), one S(12), one S(16), one S(19), one S(23), and one S(4) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(9)S6 octahedra,  an edgeedge with one Yb(1)S6 octahedra,  an edgeedge with one Yb(10)S6 octahedra,  an edgeedge with one Yb(11)S6 octahedra,  an edgeedge with one Yb(13)S6 octahedra,  an edgeedge with one Yb(5)S6 octahedra,  an edgeedge with one Yb(8)S6 octahedra, and  a faceface with one Yb(16)S7 square pyramid. The corner-sharing octahedral tilt angles are 3°. In the seventh Yb site, Yb(7) is bonded to one S(14), one S(17), one S(21), one S(27), one S(29), and one S(7) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(12)S6 octahedra,  an edgeedge with one Yb(11)S6 octahedra,  an edgeedge with one Yb(15)S6 octahedra,  an edgeedge with one Yb(3)S6 octahedra,  an edgeedge with one Yb(5)S6 octahedra,  an edgeedge with one Yb(8)S6 octahedra,  an edgeedge with one Yb(9)S6 octahedra, and  an edgeedge with one Yb(16)S7 square pyramid. The corner-sharing octahedral tilt angles are 1°. In the eighth Yb site, Yb(8) is bonded to one S(14), one S(16), one S(19), one S(21), one S(22), and one S(3) atom to form a mixture of corner and edge-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles range from 1-7°. In the ninth Yb site, Yb(9) is bonded to one S(1), one S(17), one S(19), one S(21), one S(23), and one S(24) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(6)S6 octahedra,  an edgeedge with one Yb(10)S6 octahedra,  an edgeedge with one Yb(11)S6 octahedra,  an edgeedge with one Yb(12)S6 octahedra,  an edgeedge with one Yb(13)S6 octahedra,  an edgeedge with one Yb(5)S6 octahedra,  an edgeedge with one Yb(7)S6 octahedra,  an edgeedge with one Yb(8)S6 octahedra, and  an edgeedge with one Yb(16)S7 square pyramid. The corner-sharing octahedral tilt angles are 3°. In the tenth Yb site, Yb(10) is bonded to one S(19), one S(20), one S(22), one S(24), one S(4), and one S(9) atom to form a mixture of distorted corner and edge-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles range from 0-3°. In the eleventh Yb site, Yb(11) is bonded to one S(16), one S(21), one S(23), one S(25), one S(26), and one S(29) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(15)S6 octahedra, corners with two equivalent Yb(8)S6 octahedra,  an edgeedge with one Yb(1)S6 octahedra,  an edgeedge with one Yb(12)S6 octahedra,  an edgeedge with one Yb(13)S6 octahedra,  an edgeedge with one Yb(6)S6 octahedra,  an edgeedge with one Yb(7)S6 octahedra,  an edgeedge with one Yb(9)S6 octahedra, and  an edgeedge with one Yb(16)S7 square pyramid. The corner-sharing octahedral tilt angles range from 2-7°. In the twelfth Yb site, Yb(12) is bonded to one S(15), one S(21), one S(22), one S(24), one S(26), and one S(27) atom to form a mixture of corner and edge-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles are 1°. In the thirteenth Yb site, Yb(13) is bonded to one S(23), one S(24), one S(26), one S(28), one S(4), and one S(5) atom to form YbS6 octahedra that share corners with two equivalent Yb(10)S6 octahedra, corners with two equivalent Yb(16)S7 square pyramids,  an edgeedge with one Yb(1)S6 octahedra,  an edgeedge with one Yb(11)S6 octahedra,  an edgeedge with one Yb(12)S6 octahedra,  an edgeedge with one Yb(15)S6 octahedra,  an edgeedge with one Yb(6)S6 octahedra, and  an edgeedge with one Yb(9)S6 octahedra. The corner-sharing octahedral tilt angles range from 0-1°. In the fourteenth Yb site, Yb(14) is bonded in a 7-coordinate geometry to one S(13), one S(17), one S(24), one S(27), one S(28), one S(6), and one S(9) atom. In the fifteenth Yb site, Yb(15) is bonded to one S(18), one S(26), one S(27), one S(28), one S(29), and one S(8) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(11)S6 octahedra, corners with two equivalent Yb(3)S6 octahedra,  an edgeedge with one Yb(12)S6 octahedra,  an edgeedge with one Yb(13)S6 octahedra,  an edgeedge with one Yb(7)S6 octahedra,  an edgeedge with one Yb(16)S7 square pyramid, and  a faceface with one Yb(1)S6 octahedra. The corner-sharing octahedral tilt angles range from 2-14°. In the sixteenth Yb site, Yb(16) is bonded to one S(11), one S(12), one S(17), one S(23), one S(28), one S(29), and one S(6) atom to form a mixture of corner, edge, and face-sharing YbS7 square pyramids. The corner-sharing octahedral tilt angles range from 0-4°. There are twenty-nine inequivalent S sites. In the first S site, S(1) is bonded in a trigonal non-coplanar geometry to one Yb(9), one S(18), and one S(2) atom. In the second S site, S(2) is bonded in a distorted T-shaped geometry to one Yb(3), one Yb(4), and one S(1) atom. In the third S site, S(3) is bonded in a distorted trigonal non-coplanar geometry to one Yb(8), one S(5), and one S(6) atom. In the fourth S site, S(4) is bonded to one Yb(1), one Yb(10), one Yb(13), one Yb(2), and one Yb(6) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the fifth S site, S(5) is bonded in a distorted T-shaped geometry to one Yb(13), one Yb(2), and one S(3) atom. In the sixth S site, S(6) is bonded in a 4-coordinate geometry to one Yb(14), one Yb(16), one S(13), and one S(3) atom. In the seventh S site, S(7) is bonded in an L-shaped geometry to one Yb(7) and one S(20) atom. In the eighth S site, S(8) is bonded to one Yb(1), one Yb(15), one Yb(2), one Yb(3), and one Yb(4) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the ninth S site, S(9) is bonded to one Yb(10), one Yb(14), one Yb(2), one Yb(3), and one Yb(5) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the tenth S site, S(10) is bonded in a distorted T-shaped geometry to one Yb(2), one Yb(5), and one S(15) atom. In the eleventh S site, S(11) is bonded to one Yb(16), one Yb(2), one Yb(4), one Yb(5), and one Yb(6) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twelfth S site, S(12) is bonded in a distorted L-shaped geometry to one Yb(16), one Yb(6), and one S(15) atom. In the thirteenth S site, S(13) is bonded in a 3-coordinate geometry to one Yb(14), one S(25), and one S(6) atom. In the fourteenth S site, S(14) is bonded to one Yb(3), one Yb(4), one Yb(5), one Yb(7), and one Yb(8) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the fifteenth S site, S(15) is bonded in a distorted trigonal non-coplanar geometry to one Yb(12), one S(10), and one S(12) atom. In the sixteenth S site, S(16) is bonded to one Yb(1), one Yb(11), one Yb(4), one Yb(6), and one Yb(8) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the seventeenth S site, S(17) is bonded to one Yb(14), one Yb(16), one Yb(5), one Yb(7), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the eighteenth S site, S(18) is bonded in a distorted T-shaped geometry to one Yb(1), one Yb(15), and one S(1) atom. In the nineteenth S site, S(19) is bonded to one Yb(10), one Yb(5), one Yb(6), one Yb(8), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twentieth S site, S(20) is bonded in an L-shaped geometry to one Yb(10) and one S(7) atom. In the twenty-first S site, S(21) is bonded to one Yb(11), one Yb(12), one Yb(7), one Yb(8), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-second S site, S(22) is bonded to one Yb(1), one Yb(10), one Yb(12), one Yb(3), and one Yb(8) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-third S site, S(23) is bonded to one Yb(11), one Yb(13), one Yb(16), one Yb(6), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-fourth S site, S(24) is bonded to one Yb(10), one Yb(12), one Yb(13), one Yb(14), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-fifth S site, S(25) is bonded in a 3-coordinate geometry to one Yb(11), one Yb(4), and one S(13) atom. In the twenty-sixth S site, S(26) is bonded to one Yb(1), one Yb(11), one Yb(12), one Yb(13), and one Yb(15) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-seventh S site, S(27) is bonded to one Yb(12), one Yb(14), one Yb(15), one Yb(3), and one Yb(7) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-eighth S site, S(28) is bonded to one Yb(13), one Yb(14), one Yb(15), one Yb(16), and one Yb(2) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-ninth S site, S(29) is bonded to one Yb(11), one Yb(15), one Yb(16), one Yb(4), and one Yb(7) atom to form a mixture of corner and edge-sharing SYb5 square pyramids.
Yb16S29 crystallizes in the triclinic P1 space group. There are sixteen inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to one S(16), one S(18), one S(22), one S(26), one S(4), and one S(8) atom to form a mixture of distorted corner, edge, and face-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles are 1°. The Yb(1)-S(16) bond length is 2.77 Å. The Yb(1)-S(18) bond length is 3.33 Å. The Yb(1)-S(22) bond length is 2.79 Å. The Yb(1)-S(26) bond length is 2.77 Å. The Yb(1)-S(4) bond length is 2.78 Å. The Yb(1)-S(8) bond length is 2.80 Å. In the second Yb site, Yb(2) is bonded in a 7-coordinate geometry to one S(10), one S(11), one S(28), one S(4), one S(5), one S(8), and one S(9) atom. The Yb(2)-S(10) bond length is 3.30 Å. The Yb(2)-S(11) bond length is 2.79 Å. The Yb(2)-S(28) bond length is 2.82 Å. The Yb(2)-S(4) bond length is 2.80 Å. The Yb(2)-S(5) bond length is 3.10 Å. The Yb(2)-S(8) bond length is 2.79 Å. The Yb(2)-S(9) bond length is 2.79 Å. In the third Yb site, Yb(3) is bonded to one S(14), one S(2), one S(22), one S(27), one S(8), and one S(9) atom to form a mixture of distorted corner and edge-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles range from 1-14°. The Yb(3)-S(14) bond length is 2.77 Å. The Yb(3)-S(2) bond length is 3.22 Å. The Yb(3)-S(22) bond length is 2.79 Å. The Yb(3)-S(27) bond length is 2.80 Å. The Yb(3)-S(8) bond length is 2.79 Å. The Yb(3)-S(9) bond length is 2.82 Å. In the fourth Yb site, Yb(4) is bonded in a 6-coordinate geometry to one S(11), one S(14), one S(16), one S(2), one S(25), one S(29), and one S(8) atom. The Yb(4)-S(11) bond length is 2.81 Å. The Yb(4)-S(14) bond length is 2.79 Å. The Yb(4)-S(16) bond length is 2.81 Å. The Yb(4)-S(2) bond length is 3.13 Å. The Yb(4)-S(25) bond length is 3.49 Å. The Yb(4)-S(29) bond length is 2.76 Å. The Yb(4)-S(8) bond length is 2.81 Å. In the fifth Yb site, Yb(5) is bonded to one S(10), one S(11), one S(14), one S(17), one S(19), and one S(9) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(10)S6 octahedra, corners with two equivalent Yb(16)S7 square pyramids,  an edgeedge with one Yb(3)S6 octahedra,  an edgeedge with one Yb(6)S6 octahedra,  an edgeedge with one Yb(7)S6 octahedra,  an edgeedge with one Yb(8)S6 octahedra, and  an edgeedge with one Yb(9)S6 octahedra. The corner-sharing octahedral tilt angles range from 1-3°. The Yb(5)-S(10) bond length is 3.10 Å. The Yb(5)-S(11) bond length is 2.81 Å. The Yb(5)-S(14) bond length is 2.81 Å. The Yb(5)-S(17) bond length is 2.79 Å. The Yb(5)-S(19) bond length is 2.79 Å. The Yb(5)-S(9) bond length is 2.76 Å. In the sixth Yb site, Yb(6) is bonded to one S(11), one S(12), one S(16), one S(19), one S(23), and one S(4) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(9)S6 octahedra,  an edgeedge with one Yb(1)S6 octahedra,  an edgeedge with one Yb(10)S6 octahedra,  an edgeedge with one Yb(11)S6 octahedra,  an edgeedge with one Yb(13)S6 octahedra,  an edgeedge with one Yb(5)S6 octahedra,  an edgeedge with one Yb(8)S6 octahedra, and  a faceface with one Yb(16)S7 square pyramid. The corner-sharing octahedral tilt angles are 3°. The Yb(6)-S(11) bond length is 2.79 Å. The Yb(6)-S(12) bond length is 3.11 Å. The Yb(6)-S(16) bond length is 2.74 Å. The Yb(6)-S(19) bond length is 2.81 Å. The Yb(6)-S(23) bond length is 2.78 Å. The Yb(6)-S(4) bond length is 2.81 Å. In the seventh Yb site, Yb(7) is bonded to one S(14), one S(17), one S(21), one S(27), one S(29), and one S(7) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(12)S6 octahedra,  an edgeedge with one Yb(11)S6 octahedra,  an edgeedge with one Yb(15)S6 octahedra,  an edgeedge with one Yb(3)S6 octahedra,  an edgeedge with one Yb(5)S6 octahedra,  an edgeedge with one Yb(8)S6 octahedra,  an edgeedge with one Yb(9)S6 octahedra, and  an edgeedge with one Yb(16)S7 square pyramid. The corner-sharing octahedral tilt angles are 1°. The Yb(7)-S(14) bond length is 2.80 Å. The Yb(7)-S(17) bond length is 2.80 Å. The Yb(7)-S(21) bond length is 2.80 Å. The Yb(7)-S(27) bond length is 2.77 Å. The Yb(7)-S(29) bond length is 2.81 Å. The Yb(7)-S(7) bond length is 3.04 Å. In the eighth Yb site, Yb(8) is bonded to one S(14), one S(16), one S(19), one S(21), one S(22), and one S(3) atom to form a mixture of corner and edge-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles range from 1-7°. The Yb(8)-S(14) bond length is 2.79 Å. The Yb(8)-S(16) bond length is 2.76 Å. The Yb(8)-S(19) bond length is 2.82 Å. The Yb(8)-S(21) bond length is 2.80 Å. The Yb(8)-S(22) bond length is 2.79 Å. The Yb(8)-S(3) bond length is 3.08 Å. In the ninth Yb site, Yb(9) is bonded to one S(1), one S(17), one S(19), one S(21), one S(23), and one S(24) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(6)S6 octahedra,  an edgeedge with one Yb(10)S6 octahedra,  an edgeedge with one Yb(11)S6 octahedra,  an edgeedge with one Yb(12)S6 octahedra,  an edgeedge with one Yb(13)S6 octahedra,  an edgeedge with one Yb(5)S6 octahedra,  an edgeedge with one Yb(7)S6 octahedra,  an edgeedge with one Yb(8)S6 octahedra, and  an edgeedge with one Yb(16)S7 square pyramid. The corner-sharing octahedral tilt angles are 3°. The Yb(9)-S(1) bond length is 3.26 Å. The Yb(9)-S(17) bond length is 2.77 Å. The Yb(9)-S(19) bond length is 2.80 Å. The Yb(9)-S(21) bond length is 2.79 Å. The Yb(9)-S(23) bond length is 2.77 Å. The Yb(9)-S(24) bond length is 2.79 Å. In the tenth Yb site, Yb(10) is bonded to one S(19), one S(20), one S(22), one S(24), one S(4), and one S(9) atom to form a mixture of distorted corner and edge-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles range from 0-3°. The Yb(10)-S(19) bond length is 2.80 Å. The Yb(10)-S(20) bond length is 3.16 Å. The Yb(10)-S(22) bond length is 2.84 Å. The Yb(10)-S(24) bond length is 2.79 Å. The Yb(10)-S(4) bond length is 2.81 Å. The Yb(10)-S(9) bond length is 2.78 Å. In the eleventh Yb site, Yb(11) is bonded to one S(16), one S(21), one S(23), one S(25), one S(26), and one S(29) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(15)S6 octahedra, corners with two equivalent Yb(8)S6 octahedra,  an edgeedge with one Yb(1)S6 octahedra,  an edgeedge with one Yb(12)S6 octahedra,  an edgeedge with one Yb(13)S6 octahedra,  an edgeedge with one Yb(6)S6 octahedra,  an edgeedge with one Yb(7)S6 octahedra,  an edgeedge with one Yb(9)S6 octahedra, and  an edgeedge with one Yb(16)S7 square pyramid. The corner-sharing octahedral tilt angles range from 2-7°. The Yb(11)-S(16) bond length is 2.80 Å. The Yb(11)-S(21) bond length is 2.81 Å. The Yb(11)-S(23) bond length is 2.82 Å. The Yb(11)-S(25) bond length is 3.04 Å. The Yb(11)-S(26) bond length is 2.80 Å. The Yb(11)-S(29) bond length is 2.79 Å. In the twelfth Yb site, Yb(12) is bonded to one S(15), one S(21), one S(22), one S(24), one S(26), and one S(27) atom to form a mixture of corner and edge-sharing YbS6 octahedra. The corner-sharing octahedral tilt angles are 1°. The Yb(12)-S(15) bond length is 3.19 Å. The Yb(12)-S(21) bond length is 2.78 Å. The Yb(12)-S(22) bond length is 2.79 Å. The Yb(12)-S(24) bond length is 2.80 Å. The Yb(12)-S(26) bond length is 2.80 Å. The Yb(12)-S(27) bond length is 2.78 Å. In the thirteenth Yb site, Yb(13) is bonded to one S(23), one S(24), one S(26), one S(28), one S(4), and one S(5) atom to form YbS6 octahedra that share corners with two equivalent Yb(10)S6 octahedra, corners with two equivalent Yb(16)S7 square pyramids,  an edgeedge with one Yb(1)S6 octahedra,  an edgeedge with one Yb(11)S6 octahedra,  an edgeedge with one Yb(12)S6 octahedra,  an edgeedge with one Yb(15)S6 octahedra,  an edgeedge with one Yb(6)S6 octahedra, and  an edgeedge with one Yb(9)S6 octahedra. The corner-sharing octahedral tilt angles range from 0-1°. The Yb(13)-S(23) bond length is 2.79 Å. The Yb(13)-S(24) bond length is 2.79 Å. The Yb(13)-S(26) bond length is 2.83 Å. The Yb(13)-S(28) bond length is 2.81 Å. The Yb(13)-S(4) bond length is 2.76 Å. The Yb(13)-S(5) bond length is 3.05 Å. In the fourteenth Yb site, Yb(14) is bonded in a 7-coordinate geometry to one S(13), one S(17), one S(24), one S(27), one S(28), one S(6), and one S(9) atom. The Yb(14)-S(13) bond length is 3.16 Å. The Yb(14)-S(17) bond length is 2.78 Å. The Yb(14)-S(24) bond length is 2.80 Å. The Yb(14)-S(27) bond length is 2.79 Å. The Yb(14)-S(28) bond length is 2.78 Å. The Yb(14)-S(6) bond length is 3.33 Å. The Yb(14)-S(9) bond length is 2.80 Å. In the fifteenth Yb site, Yb(15) is bonded to one S(18), one S(26), one S(27), one S(28), one S(29), and one S(8) atom to form distorted YbS6 octahedra that share corners with two equivalent Yb(11)S6 octahedra, corners with two equivalent Yb(3)S6 octahedra,  an edgeedge with one Yb(12)S6 octahedra,  an edgeedge with one Yb(13)S6 octahedra,  an edgeedge with one Yb(7)S6 octahedra,  an edgeedge with one Yb(16)S7 square pyramid, and  a faceface with one Yb(1)S6 octahedra. The corner-sharing octahedral tilt angles range from 2-14°. The Yb(15)-S(18) bond length is 3.10 Å. The Yb(15)-S(26) bond length is 2.78 Å. The Yb(15)-S(27) bond length is 2.81 Å. The Yb(15)-S(28) bond length is 2.79 Å. The Yb(15)-S(29) bond length is 2.77 Å. The Yb(15)-S(8) bond length is 2.80 Å. In the sixteenth Yb site, Yb(16) is bonded to one S(11), one S(12), one S(17), one S(23), one S(28), one S(29), and one S(6) atom to form a mixture of corner, edge, and face-sharing YbS7 square pyramids. The corner-sharing octahedral tilt angles range from 0-4°. The Yb(16)-S(11) bond length is 2.77 Å. The Yb(16)-S(12) bond length is 3.59 Å. The Yb(16)-S(17) bond length is 2.78 Å. The Yb(16)-S(23) bond length is 2.76 Å. The Yb(16)-S(28) bond length is 2.78 Å. The Yb(16)-S(29) bond length is 2.75 Å. The Yb(16)-S(6) bond length is 3.60 Å. There are twenty-nine inequivalent S sites. In the first S site, S(1) is bonded in a trigonal non-coplanar geometry to one Yb(9), one S(18), and one S(2) atom. The S(1)-S(18) bond length is 1.99 Å. The S(1)-S(2) bond length is 1.98 Å. In the second S site, S(2) is bonded in a distorted T-shaped geometry to one Yb(3), one Yb(4), and one S(1) atom. In the third S site, S(3) is bonded in a distorted trigonal non-coplanar geometry to one Yb(8), one S(5), and one S(6) atom. The S(3)-S(5) bond length is 2.01 Å. The S(3)-S(6) bond length is 2.11 Å. In the fourth S site, S(4) is bonded to one Yb(1), one Yb(10), one Yb(13), one Yb(2), and one Yb(6) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the fifth S site, S(5) is bonded in a distorted T-shaped geometry to one Yb(13), one Yb(2), and one S(3) atom. In the sixth S site, S(6) is bonded in a 4-coordinate geometry to one Yb(14), one Yb(16), one S(13), and one S(3) atom. The S(6)-S(13) bond length is 2.15 Å. In the seventh S site, S(7) is bonded in an L-shaped geometry to one Yb(7) and one S(20) atom. The S(7)-S(20) bond length is 1.94 Å. In the eighth S site, S(8) is bonded to one Yb(1), one Yb(15), one Yb(2), one Yb(3), and one Yb(4) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the ninth S site, S(9) is bonded to one Yb(10), one Yb(14), one Yb(2), one Yb(3), and one Yb(5) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the tenth S site, S(10) is bonded in a distorted T-shaped geometry to one Yb(2), one Yb(5), and one S(15) atom. The S(10)-S(15) bond length is 2.00 Å. In the eleventh S site, S(11) is bonded to one Yb(16), one Yb(2), one Yb(4), one Yb(5), and one Yb(6) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twelfth S site, S(12) is bonded in a distorted L-shaped geometry to one Yb(16), one Yb(6), and one S(15) atom. The S(12)-S(15) bond length is 1.98 Å. In the thirteenth S site, S(13) is bonded in a 3-coordinate geometry to one Yb(14), one S(25), and one S(6) atom. The S(13)-S(25) bond length is 1.96 Å. In the fourteenth S site, S(14) is bonded to one Yb(3), one Yb(4), one Yb(5), one Yb(7), and one Yb(8) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the fifteenth S site, S(15) is bonded in a distorted trigonal non-coplanar geometry to one Yb(12), one S(10), and one S(12) atom. In the sixteenth S site, S(16) is bonded to one Yb(1), one Yb(11), one Yb(4), one Yb(6), and one Yb(8) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the seventeenth S site, S(17) is bonded to one Yb(14), one Yb(16), one Yb(5), one Yb(7), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the eighteenth S site, S(18) is bonded in a distorted T-shaped geometry to one Yb(1), one Yb(15), and one S(1) atom. In the nineteenth S site, S(19) is bonded to one Yb(10), one Yb(5), one Yb(6), one Yb(8), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twentieth S site, S(20) is bonded in an L-shaped geometry to one Yb(10) and one S(7) atom. In the twenty-first S site, S(21) is bonded to one Yb(11), one Yb(12), one Yb(7), one Yb(8), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-second S site, S(22) is bonded to one Yb(1), one Yb(10), one Yb(12), one Yb(3), and one Yb(8) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-third S site, S(23) is bonded to one Yb(11), one Yb(13), one Yb(16), one Yb(6), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-fourth S site, S(24) is bonded to one Yb(10), one Yb(12), one Yb(13), one Yb(14), and one Yb(9) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-fifth S site, S(25) is bonded in a 3-coordinate geometry to one Yb(11), one Yb(4), and one S(13) atom. In the twenty-sixth S site, S(26) is bonded to one Yb(1), one Yb(11), one Yb(12), one Yb(13), and one Yb(15) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-seventh S site, S(27) is bonded to one Yb(12), one Yb(14), one Yb(15), one Yb(3), and one Yb(7) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-eighth S site, S(28) is bonded to one Yb(13), one Yb(14), one Yb(15), one Yb(16), and one Yb(2) atom to form a mixture of corner and edge-sharing SYb5 square pyramids. In the twenty-ninth S site, S(29) is bonded to one Yb(11), one Yb(15), one Yb(16), one Yb(4), and one Yb(7) atom to form a mixture of corner and edge-sharing SYb5 square pyramids.