DyC7H6SO8 crystallizes in the monoclinic C2/c space group. There are two inequivalent Dy sites. In the first Dy site, Dy(1) is bonded in a 8-coordinate geometry to two equivalent O(1), two equivalent O(4), two equivalent O(5), and two equivalent O(6) atoms. Both Dy(1)-O(1) bond lengths are 2.26 Å. Both Dy(1)-O(4) bond lengths are 2.36 Å. Both Dy(1)-O(5) bond lengths are 2.42 Å. Both Dy(1)-O(6) bond lengths are 2.40 Å. In the second Dy site, Dy(2) is bonded in a 8-coordinate geometry to two equivalent O(2), two equivalent O(3), two equivalent O(7), and two equivalent O(8) atoms. Both Dy(2)-O(2) bond lengths are 2.33 Å. Both Dy(2)-O(3) bond lengths are 2.30 Å. Both Dy(2)-O(7) bond lengths are 2.47 Å. Both Dy(2)-O(8) bond lengths are 2.38 Å. There are seven inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(5), and one S(1) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-C(5) bond length is 1.47 Å. The C(1)-S(1) bond length is 1.72 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1) and one H(5) atom. The C(2)-H(5) bond length is 1.09 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(4) and one H(6) atom. The C(3)-C(4) bond length is 1.39 Å. The C(3)-H(6) bond length is 1.09 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(6), and one S(1) atom. The C(4)-C(6) bond length is 1.47 Å. The C(4)-S(1) bond length is 1.72 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(1), and one O(2) atom. The C(5)-O(1) bond length is 1.27 Å. The C(5)-O(2) bond length is 1.28 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(6)-O(3) bond length is 1.28 Å. The C(6)-O(4) bond length is 1.27 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one O(5) and one O(6) atom. The C(7)-O(5) bond length is 1.26 Å. The C(7)-O(6) bond length is 1.27 Å. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(7) atom. The H(1)-O(7) bond length is 0.97 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(7) atom. The H(2)-O(7) bond length is 0.99 Å. In the third H site, H(3) is bonded in a single-bond geometry to one O(8) atom. The H(3)-O(8) bond length is 0.99 Å. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(8) atom. The H(4)-O(8) bond length is 0.98 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(2) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(3) atom. S(1) is bonded in an L-shaped geometry to one C(1) and one C(4) atom. There are eight inequivalent O sites. In the first O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Dy(2) and one C(6) atom. In the second O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Dy(1) and one C(6) atom. In the third O site, O(5) is bonded in a distorted single-bond geometry to one Dy(1) and one C(7) atom. In the fourth O site, O(6) is bonded in a 1-coordinate geometry to one Dy(1) and one C(7) atom. In the fifth O site, O(7) is bonded in a water-like geometry to one Dy(2), one H(1), and one H(2) atom. In the sixth O site, O(8) is bonded in a water-like geometry to one Dy(2), one H(3), and one H(4) atom. In the seventh O site, O(1) is bonded in a bent 150 degrees geometry to one Dy(1) and one C(5) atom. In the eighth O site, O(2) is bonded in a 2-coordinate geometry to one Dy(2) and one C(5) atom. Linkers: 1 [O]C(=O)C([O])=O ,4 [O]C(=O)c1ccc(C([O])=O)s1. Metal clusters: 4 [Dy]. The MOF has largest included sphere 3.33 A, density 2.45 g/cm3, surface area 2508.71 m2/g, accessible volume 0.08 cm3/g