Yb3Se4 crystallizes in the orthorhombic Cmmm space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to two equivalent Se(2) and four equivalent Se(1) atoms to form a mixture of corner and edge-sharing YbSe6 octahedra. The corner-sharing octahedral tilt angles range from 1-3°. In the second Yb site, Yb(2) is bonded to two equivalent Se(1) and four equivalent Se(2) atoms to form edge-sharing YbSe6 octahedra. There are two inequivalent Se sites. In the first Se site, Se(1) is bonded to one Yb(2) and four equivalent Yb(1) atoms to form a mixture of corner and edge-sharing SeYb5 square pyramids. In the second Se site, Se(2) is bonded in a rectangular see-saw-like geometry to two equivalent Yb(1) and two equivalent Yb(2) atoms.
Yb3Se4 crystallizes in the orthorhombic Cmmm space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded to two equivalent Se(2) and four equivalent Se(1) atoms to form a mixture of corner and edge-sharing YbSe6 octahedra. The corner-sharing octahedral tilt angles range from 1-3°. Both Yb(1)-Se(2) bond lengths are 2.95 Å. All Yb(1)-Se(1) bond lengths are 2.93 Å. In the second Yb site, Yb(2) is bonded to two equivalent Se(1) and four equivalent Se(2) atoms to form edge-sharing YbSe6 octahedra. Both Yb(2)-Se(1) bond lengths are 2.91 Å. All Yb(2)-Se(2) bond lengths are 2.87 Å. There are two inequivalent Se sites. In the first Se site, Se(1) is bonded to one Yb(2) and four equivalent Yb(1) atoms to form a mixture of corner and edge-sharing SeYb5 square pyramids. In the second Se site, Se(2) is bonded in a rectangular see-saw-like geometry to two equivalent Yb(1) and two equivalent Yb(2) atoms.