Yb2ZnS4 is Spinel-like structured and crystallizes in the orthorhombic Pnma space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to two equivalent S(1), two equivalent S(2), and two equivalent S(3) atoms to form YbS6 octahedra that share corners with four equivalent Yb(2)S6 octahedra, corners with two equivalent Zn(1)S4 tetrahedra, edges with two equivalent Yb(1)S6 octahedra, edges with two equivalent Yb(2)S6 octahedra, and edges with two equivalent Zn(1)S4 tetrahedra. The corner-sharing octahedral tilt angles range from 53-58°. In the second Yb site, Yb(2) is bonded to one S(1), one S(2), and four equivalent S(3) atoms to form YbS6 octahedra that share corners with four equivalent Yb(1)S6 octahedra, corners with four equivalent Yb(2)S6 octahedra, corners with four equivalent Zn(1)S4 tetrahedra, edges with two equivalent Yb(1)S6 octahedra, and  an edgeedge with one Zn(1)S4 tetrahedra. The corner-sharing octahedral tilt angles range from 48-58°. Zn(1) is bonded to one S(1), one S(2), and two equivalent S(3) atoms to form ZnS4 tetrahedra that share corners with two equivalent Yb(1)S6 octahedra, corners with four equivalent Yb(2)S6 octahedra,  an edgeedge with one Yb(2)S6 octahedra, and edges with two equivalent Yb(1)S6 octahedra. The corner-sharing octahedral tilt angles range from 56-59°. There are three inequivalent S sites. In the first S site, S(1) is bonded to one Yb(2), two equivalent Yb(1), and one Zn(1) atom to form distorted corner-sharing SYb3Zn trigonal pyramids. In the second S site, S(2) is bonded in a rectangular see-saw-like geometry to one Yb(2), two equivalent Yb(1), and one Zn(1) atom. In the third S site, S(3) is bonded in a rectangular see-saw-like geometry to one Yb(1), two equivalent Yb(2), and one Zn(1) atom.
Yb2ZnS4 is Spinel-like structured and crystallizes in the orthorhombic Pnma space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to two equivalent S(1), two equivalent S(2), and two equivalent S(3) atoms to form YbS6 octahedra that share corners with four equivalent Yb(2)S6 octahedra, corners with two equivalent Zn(1)S4 tetrahedra, edges with two equivalent Yb(1)S6 octahedra, edges with two equivalent Yb(2)S6 octahedra, and edges with two equivalent Zn(1)S4 tetrahedra. The corner-sharing octahedral tilt angles range from 53-58°. Both Yb(1)-S(1) bond lengths are 2.81 Å. Both Yb(1)-S(2) bond lengths are 2.75 Å. Both Yb(1)-S(3) bond lengths are 2.80 Å. In the second Yb site, Yb(2) is bonded to one S(1), one S(2), and four equivalent S(3) atoms to form YbS6 octahedra that share corners with four equivalent Yb(1)S6 octahedra, corners with four equivalent Yb(2)S6 octahedra, corners with four equivalent Zn(1)S4 tetrahedra, edges with two equivalent Yb(1)S6 octahedra, and  an edgeedge with one Zn(1)S4 tetrahedra. The corner-sharing octahedral tilt angles range from 48-58°. The Yb(2)-S(1) bond length is 2.81 Å. The Yb(2)-S(2) bond length is 2.77 Å. There are two shorter (2.81 Å) and two longer (2.82 Å) Yb(2)-S(3) bond lengths. Zn(1) is bonded to one S(1), one S(2), and two equivalent S(3) atoms to form ZnS4 tetrahedra that share corners with two equivalent Yb(1)S6 octahedra, corners with four equivalent Yb(2)S6 octahedra,  an edgeedge with one Yb(2)S6 octahedra, and edges with two equivalent Yb(1)S6 octahedra. The corner-sharing octahedral tilt angles range from 56-59°. The Zn(1)-S(1) bond length is 2.28 Å. The Zn(1)-S(2) bond length is 2.37 Å. Both Zn(1)-S(3) bond lengths are 2.34 Å. There are three inequivalent S sites. In the first S site, S(1) is bonded to one Yb(2), two equivalent Yb(1), and one Zn(1) atom to form distorted corner-sharing SYb3Zn trigonal pyramids. In the second S site, S(2) is bonded in a rectangular see-saw-like geometry to one Yb(2), two equivalent Yb(1), and one Zn(1) atom. In the third S site, S(3) is bonded in a rectangular see-saw-like geometry to one Yb(1), two equivalent Yb(2), and one Zn(1) atom.