Re3(PbSe3)2 crystallizes in the monoclinic C2/c space group. There are three inequivalent Re sites. In the first Re site, Re(1) is bonded to one Se(1), one Se(2), one Se(3), one Se(4), and one Se(5) atom to form a mixture of distorted corner and edge-sharing ReSe5 square pyramids. In the second Re site, Re(2) is bonded to one Se(1), one Se(2), one Se(3), one Se(4), and one Se(5) atom to form a mixture of distorted corner and edge-sharing ReSe5 square pyramids. In the third Re site, Re(3) is bonded to one Se(1), one Se(3), one Se(4), one Se(5), and one Se(6) atom to form distorted edge-sharing ReSe5 square pyramids. There are three inequivalent Pb sites. In the first Pb site, Pb(1) is bonded in a water-like geometry to two equivalent Se(2) atoms. In the second Pb site, Pb(2) is bonded in a 2-coordinate geometry to one Se(2) and one Se(6) atom. In the third Pb site, Pb(3) is bonded in a distorted L-shaped geometry to two equivalent Se(2), two equivalent Se(3), and two equivalent Se(6) atoms. There are six inequivalent Se sites. In the first Se site, Se(5) is bonded in a 3-coordinate geometry to one Re(1), one Re(2), and one Re(3) atom. In the second Se site, Se(1) is bonded in a 3-coordinate geometry to one Re(1), one Re(2), and one Re(3) atom. In the third Se site, Se(2) is bonded in a 5-coordinate geometry to one Re(1), one Re(2), one Pb(1), one Pb(2), and one Pb(3) atom. In the fourth Se site, Se(3) is bonded in a 3-coordinate geometry to one Re(1), one Re(2), one Re(3), and one Pb(3) atom. In the fifth Se site, Se(4) is bonded in a 3-coordinate geometry to one Re(1), one Re(2), and one Re(3) atom. In the sixth Se site, Se(6) is bonded in a 3-coordinate geometry to one Re(3), one Pb(2), and one Pb(3) atom.
Re3(PbSe3)2 crystallizes in the monoclinic C2/c space group. There are three inequivalent Re sites. In the first Re site, Re(1) is bonded to one Se(1), one Se(2), one Se(3), one Se(4), and one Se(5) atom to form a mixture of distorted corner and edge-sharing ReSe5 square pyramids. The Re(1)-Se(1) bond length is 2.56 Å. The Re(1)-Se(2) bond length is 2.73 Å. The Re(1)-Se(3) bond length is 2.54 Å. The Re(1)-Se(4) bond length is 2.58 Å. The Re(1)-Se(5) bond length is 2.57 Å. In the second Re site, Re(2) is bonded to one Se(1), one Se(2), one Se(3), one Se(4), and one Se(5) atom to form a mixture of distorted corner and edge-sharing ReSe5 square pyramids. The Re(2)-Se(1) bond length is 2.53 Å. The Re(2)-Se(2) bond length is 2.70 Å. The Re(2)-Se(3) bond length is 2.54 Å. The Re(2)-Se(4) bond length is 2.60 Å. The Re(2)-Se(5) bond length is 2.54 Å. In the third Re site, Re(3) is bonded to one Se(1), one Se(3), one Se(4), one Se(5), and one Se(6) atom to form distorted edge-sharing ReSe5 square pyramids. The Re(3)-Se(1) bond length is 2.54 Å. The Re(3)-Se(3) bond length is 2.56 Å. The Re(3)-Se(4) bond length is 2.58 Å. The Re(3)-Se(5) bond length is 2.57 Å. The Re(3)-Se(6) bond length is 2.58 Å. There are three inequivalent Pb sites. In the first Pb site, Pb(1) is bonded in a water-like geometry to two equivalent Se(2) atoms. Both Pb(1)-Se(2) bond lengths are 3.10 Å. In the second Pb site, Pb(2) is bonded in a 2-coordinate geometry to one Se(2) and one Se(6) atom. The Pb(2)-Se(2) bond length is 3.09 Å. The Pb(2)-Se(6) bond length is 2.92 Å. In the third Pb site, Pb(3) is bonded in a distorted L-shaped geometry to two equivalent Se(2), two equivalent Se(3), and two equivalent Se(6) atoms. Both Pb(3)-Se(2) bond lengths are 3.32 Å. Both Pb(3)-Se(3) bond lengths are 3.31 Å. Both Pb(3)-Se(6) bond lengths are 2.80 Å. There are six inequivalent Se sites. In the first Se site, Se(5) is bonded in a 3-coordinate geometry to one Re(1), one Re(2), and one Re(3) atom. In the second Se site, Se(1) is bonded in a 3-coordinate geometry to one Re(1), one Re(2), and one Re(3) atom. In the third Se site, Se(2) is bonded in a 5-coordinate geometry to one Re(1), one Re(2), one Pb(1), one Pb(2), and one Pb(3) atom. In the fourth Se site, Se(3) is bonded in a 3-coordinate geometry to one Re(1), one Re(2), one Re(3), and one Pb(3) atom. In the fifth Se site, Se(4) is bonded in a 3-coordinate geometry to one Re(1), one Re(2), and one Re(3) atom. In the sixth Se site, Se(6) is bonded in a 3-coordinate geometry to one Re(3), one Pb(2), and one Pb(3) atom.