Yb2PbS4 crystallizes in the orthorhombic Pnma space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 6-coordinate geometry to one S(2), one S(3), two equivalent S(1), and three equivalent S(4) atoms. In the second Yb site, Yb(2) is bonded to one S(1), two equivalent S(3), and three equivalent S(2) atoms to form distorted edge-sharing YbS6 octahedra. Pb(1) is bonded in a 4-coordinate geometry to two equivalent S(1) and two equivalent S(3) atoms. There are four inequivalent S sites. In the first S site, S(1) is bonded in a 5-coordinate geometry to one Yb(2), two equivalent Yb(1), and two equivalent Pb(1) atoms. In the second S site, S(2) is bonded to one Yb(1), three equivalent Yb(2), and one S(4) atom to form a mixture of distorted corner and edge-sharing SYb4S square pyramids. In the third S site, S(3) is bonded in a 5-coordinate geometry to one Yb(1), two equivalent Yb(2), and two equivalent Pb(1) atoms. In the fourth S site, S(4) is bonded in a 4-coordinate geometry to three equivalent Yb(1) and one S(2) atom.
Yb2PbS4 crystallizes in the orthorhombic Pnma space group. There are two inequivalent Yb sites. In the first Yb site, Yb(1) is bonded in a 6-coordinate geometry to one S(2), one S(3), two equivalent S(1), and three equivalent S(4) atoms. The Yb(1)-S(2) bond length is 3.24 Å. The Yb(1)-S(3) bond length is 2.90 Å. Both Yb(1)-S(1) bond lengths are 2.76 Å. There is one shorter (2.86 Å) and two longer (2.96 Å) Yb(1)-S(4) bond lengths. In the second Yb site, Yb(2) is bonded to one S(1), two equivalent S(3), and three equivalent S(2) atoms to form distorted edge-sharing YbS6 octahedra. The Yb(2)-S(1) bond length is 2.68 Å. Both Yb(2)-S(3) bond lengths are 2.73 Å. There are two shorter (2.92 Å) and one longer (3.51 Å) Yb(2)-S(2) bond length. Pb(1) is bonded in a 4-coordinate geometry to two equivalent S(1) and two equivalent S(3) atoms. Both Pb(1)-S(1) bond lengths are 2.90 Å. There is one shorter (2.86 Å) and one longer (2.93 Å) Pb(1)-S(3) bond length. There are four inequivalent S sites. In the first S site, S(1) is bonded in a 5-coordinate geometry to one Yb(2), two equivalent Yb(1), and two equivalent Pb(1) atoms. In the second S site, S(2) is bonded to one Yb(1), three equivalent Yb(2), and one S(4) atom to form a mixture of distorted corner and edge-sharing SYb4S square pyramids. The S(2)-S(4) bond length is 2.14 Å. In the third S site, S(3) is bonded in a 5-coordinate geometry to one Yb(1), two equivalent Yb(2), and two equivalent Pb(1) atoms. In the fourth S site, S(4) is bonded in a 4-coordinate geometry to three equivalent Yb(1) and one S(2) atom.