MgYb2S4 crystallizes in the orthorhombic Pnma space group. Mg(1) is bonded in a 4-coordinate geometry to one S(3), two equivalent S(1), and three equivalent S(2) atoms. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 7-coordinate geometry to one S(3), two equivalent S(2), and four equivalent S(1) atoms. In the second Yb site, Yb(2) is bonded to one S(2), two equivalent S(1), and three equivalent S(3) atoms to form a mixture of distorted edge and corner-sharing YbS6 pentagonal pyramids. There are three inequivalent S sites. In the first S site, S(1) is bonded in a 5-coordinate geometry to one Mg(1), one Yb(2), two equivalent Yb(1), and one S(1) atom. In the second S site, S(2) is bonded in a 6-coordinate geometry to three equivalent Mg(1), one Yb(2), and two equivalent Yb(1) atoms. In the third S site, S(3) is bonded in a 5-coordinate geometry to one Mg(1), one Yb(1), and three equivalent Yb(2) atoms.
MgYb2S4 crystallizes in the orthorhombic Pnma space group. Mg(1) is bonded in a 4-coordinate geometry to one S(3), two equivalent S(1), and three equivalent S(2) atoms. The Mg(1)-S(3) bond length is 2.48 Å. Both Mg(1)-S(1) bond lengths are 2.61 Å. There is one shorter (2.39 Å) and two longer (3.09 Å) Mg(1)-S(2) bond lengths. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 7-coordinate geometry to one S(3), two equivalent S(2), and four equivalent S(1) atoms. The Yb(1)-S(3) bond length is 2.94 Å. Both Yb(1)-S(2) bond lengths are 3.11 Å. There are two shorter (2.84 Å) and two longer (2.89 Å) Yb(1)-S(1) bond lengths. In the second Yb site, Yb(2) is bonded to one S(2), two equivalent S(1), and three equivalent S(3) atoms to form a mixture of distorted edge and corner-sharing YbS6 pentagonal pyramids. The Yb(2)-S(2) bond length is 2.79 Å. Both Yb(2)-S(1) bond lengths are 2.88 Å. There are two shorter (2.74 Å) and one longer (2.87 Å) Yb(2)-S(3) bond length. There are three inequivalent S sites. In the first S site, S(1) is bonded in a 5-coordinate geometry to one Mg(1), one Yb(2), two equivalent Yb(1), and one S(1) atom. The S(1)-S(1) bond length is 2.08 Å. In the second S site, S(2) is bonded in a 6-coordinate geometry to three equivalent Mg(1), one Yb(2), and two equivalent Yb(1) atoms. In the third S site, S(3) is bonded in a 5-coordinate geometry to one Mg(1), one Yb(1), and three equivalent Yb(2) atoms.