Rb2(ReS2)3 crystallizes in the monoclinic C2/c space group. There are three inequivalent Rb sites. In the first Rb site, Rb(1) is bonded in a 6-coordinate geometry to two equivalent S(2), two equivalent S(4), and two equivalent S(5) atoms. In the second Rb site, Rb(2) is bonded in a 8-coordinate geometry to one S(2), one S(4), two equivalent S(3), two equivalent S(5), and two equivalent S(6) atoms. In the third Rb site, Rb(3) is bonded in a 8-coordinate geometry to two equivalent S(1), two equivalent S(4), two equivalent S(5), and two equivalent S(6) atoms. There are three inequivalent Re sites. In the first Re site, Re(1) is bonded to one S(1), one S(2), one S(3), one S(5), and one S(6) atom to form edge-sharing ReS5 square pyramids. In the second Re site, Re(2) is bonded to one S(1), one S(2), one S(3), one S(4), and one S(5) atom to form a mixture of edge and corner-sharing ReS5 square pyramids. In the third Re site, Re(3) is bonded to one S(1), one S(2), one S(3), one S(4), and one S(5) atom to form a mixture of edge and corner-sharing ReS5 square pyramids. There are six inequivalent S sites. In the first S site, S(1) is bonded in a 4-coordinate geometry to one Rb(3), one Re(1), one Re(2), and one Re(3) atom. In the second S site, S(2) is bonded in a 5-coordinate geometry to one Rb(1), one Rb(2), one Re(1), one Re(2), and one Re(3) atom. In the third S site, S(3) is bonded to two equivalent Rb(2), one Re(1), one Re(2), and one Re(3) atom to form distorted edge-sharing SRb2Re3 trigonal bipyramids. In the fourth S site, S(4) is bonded in a 5-coordinate geometry to one Rb(1), one Rb(2), one Rb(3), one Re(2), and one Re(3) atom. In the fifth S site, S(5) is bonded in a 7-coordinate geometry to one Rb(1), one Rb(3), two equivalent Rb(2), one Re(1), one Re(2), and one Re(3) atom. In the sixth S site, S(6) is bonded in a 5-coordinate geometry to one Rb(3), two equivalent Rb(2), one Re(1), and one S(6) atom.
Rb2(ReS2)3 crystallizes in the monoclinic C2/c space group. There are three inequivalent Rb sites. In the first Rb site, Rb(1) is bonded in a 6-coordinate geometry to two equivalent S(2), two equivalent S(4), and two equivalent S(5) atoms. Both Rb(1)-S(2) bond lengths are 3.28 Å. Both Rb(1)-S(4) bond lengths are 3.26 Å. Both Rb(1)-S(5) bond lengths are 3.54 Å. In the second Rb site, Rb(2) is bonded in a 8-coordinate geometry to one S(2), one S(4), two equivalent S(3), two equivalent S(5), and two equivalent S(6) atoms. The Rb(2)-S(2) bond length is 3.33 Å. The Rb(2)-S(4) bond length is 3.26 Å. There is one shorter (3.17 Å) and one longer (3.26 Å) Rb(2)-S(3) bond length. There is one shorter (3.65 Å) and one longer (3.79 Å) Rb(2)-S(5) bond length. There is one shorter (3.33 Å) and one longer (3.36 Å) Rb(2)-S(6) bond length. In the third Rb site, Rb(3) is bonded in a 8-coordinate geometry to two equivalent S(1), two equivalent S(4), two equivalent S(5), and two equivalent S(6) atoms. Both Rb(3)-S(1) bond lengths are 3.20 Å. Both Rb(3)-S(4) bond lengths are 3.35 Å. Both Rb(3)-S(5) bond lengths are 3.54 Å. Both Rb(3)-S(6) bond lengths are 3.32 Å. There are three inequivalent Re sites. In the first Re site, Re(1) is bonded to one S(1), one S(2), one S(3), one S(5), and one S(6) atom to form edge-sharing ReS5 square pyramids. The Re(1)-S(1) bond length is 2.40 Å. The Re(1)-S(2) bond length is 2.41 Å. The Re(1)-S(3) bond length is 2.42 Å. The Re(1)-S(5) bond length is 2.45 Å. The Re(1)-S(6) bond length is 2.51 Å. In the second Re site, Re(2) is bonded to one S(1), one S(2), one S(3), one S(4), and one S(5) atom to form a mixture of edge and corner-sharing ReS5 square pyramids. The Re(2)-S(1) bond length is 2.43 Å. The Re(2)-S(2) bond length is 2.39 Å. The Re(2)-S(3) bond length is 2.39 Å. The Re(2)-S(4) bond length is 2.48 Å. The Re(2)-S(5) bond length is 2.44 Å. In the third Re site, Re(3) is bonded to one S(1), one S(2), one S(3), one S(4), and one S(5) atom to form a mixture of edge and corner-sharing ReS5 square pyramids. The Re(3)-S(1) bond length is 2.38 Å. The Re(3)-S(2) bond length is 2.42 Å. The Re(3)-S(3) bond length is 2.43 Å. The Re(3)-S(4) bond length is 2.49 Å. The Re(3)-S(5) bond length is 2.45 Å. There are six inequivalent S sites. In the first S site, S(1) is bonded in a 4-coordinate geometry to one Rb(3), one Re(1), one Re(2), and one Re(3) atom. In the second S site, S(2) is bonded in a 5-coordinate geometry to one Rb(1), one Rb(2), one Re(1), one Re(2), and one Re(3) atom. In the third S site, S(3) is bonded to two equivalent Rb(2), one Re(1), one Re(2), and one Re(3) atom to form distorted edge-sharing SRb2Re3 trigonal bipyramids. In the fourth S site, S(4) is bonded in a 5-coordinate geometry to one Rb(1), one Rb(2), one Rb(3), one Re(2), and one Re(3) atom. In the fifth S site, S(5) is bonded in a 7-coordinate geometry to one Rb(1), one Rb(3), two equivalent Rb(2), one Re(1), one Re(2), and one Re(3) atom. In the sixth S site, S(6) is bonded in a 5-coordinate geometry to one Rb(3), two equivalent Rb(2), one Re(1), and one S(6) atom. The S(6)-S(6) bond length is 2.13 Å.