KDyC9H2SO9 crystallizes in the monoclinic C2/c space group. K(1) is bonded in a 7-coordinate geometry to one O(4), one O(8), one O(9), two equivalent O(1), and two equivalent O(2) atoms. The K(1)-O(4) bond length is 2.81 Å. The K(1)-O(8) bond length is 2.77 Å. The K(1)-O(9) bond length is 3.31 Å. There is one shorter (2.96 Å) and one longer (3.12 Å) K(1)-O(1) bond length. There is one shorter (2.77 Å) and one longer (2.91 Å) K(1)-O(2) bond length. Dy(1) is bonded in a 7-coordinate geometry to one O(1), one O(3), one O(4), one O(5), one O(6), one O(7), and one O(8) atom. The Dy(1)-O(1) bond length is 2.45 Å. The Dy(1)-O(3) bond length is 2.52 Å. The Dy(1)-O(4) bond length is 2.46 Å. The Dy(1)-O(5) bond length is 2.45 Å. The Dy(1)-O(6) bond length is 2.43 Å. The Dy(1)-O(7) bond length is 2.32 Å. The Dy(1)-O(8) bond length is 2.46 Å. There are nine inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(4), one C(6), and one S(1) atom. The C(1)-C(4) bond length is 1.41 Å. The C(1)-C(6) bond length is 1.38 Å. The C(1)-S(1) bond length is 1.78 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(1), and one O(5) atom. The C(2)-C(3) bond length is 1.51 Å. The C(2)-O(1) bond length is 1.26 Å. The C(2)-O(5) bond length is 1.25 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(5), and one C(6) atom. The C(3)-C(5) bond length is 1.39 Å. The C(3)-C(6) bond length is 1.38 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(1), one C(8), and one C(9) atom. The C(4)-C(8) bond length is 1.38 Å. The C(4)-C(9) bond length is 1.50 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(3), one C(7), and one C(8) atom. The C(5)-C(7) bond length is 1.50 Å. The C(5)-C(8) bond length is 1.40 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(1), one C(3), and one H(1) atom. The C(6)-H(1) bond length is 0.96 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(4), and one O(8) atom. The C(7)-O(4) bond length is 1.26 Å. The C(7)-O(8) bond length is 1.26 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(4), one C(5), and one H(2) atom. The C(8)-H(2) bond length is 0.96 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(6) atom. The C(9)-O(3) bond length is 1.26 Å. The C(9)-O(6) bond length is 1.26 Å. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(6) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(8) atom. S(1) is bonded in a distorted trigonal non-coplanar geometry to one C(1), one O(2), one O(7), and one O(9) atom. The S(1)-O(2) bond length is 1.44 Å. The S(1)-O(7) bond length is 1.46 Å. The S(1)-O(9) bond length is 1.45 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to two equivalent K(1), one Dy(1), and one C(2) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to two equivalent K(1) and one S(1) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one Dy(1) and one C(9) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one K(1), one Dy(1), and one C(7) atom. In the fifth O site, O(5) is bonded in a distorted single-bond geometry to one Dy(1) and one C(2) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Dy(1) and one C(9) atom. In the seventh O site, O(7) is bonded in a bent 150 degrees geometry to one Dy(1) and one S(1) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one K(1), one Dy(1), and one C(7) atom. In the ninth O site, O(9) is bonded in a single-bond geometry to one K(1) and one S(1) atom. Linkers: 8 [O]C(=O)c1cc(C([O])=O)c(S([O])([O])[O])cc1C([O])=O. Metal clusters: 8 [K] ,8 [Dy]. The MOF has largest included sphere 6.01 A, density 1.86 g/cm3, surface area 2166.38 m2/g, accessible volume 0.15 cm3/g