K3Co2C72H78(SO3)6 crystallizes in the cubic I-43d space group. K(1) is bonded in a 4-coordinate geometry to two equivalent O(2) and two equivalent O(3) atoms. Both K(1)-O(2) bond lengths are 2.61 Å. Both K(1)-O(3) bond lengths are 2.74 Å. Co(1) is bonded in a distorted T-shaped geometry to three equivalent O(1) atoms. All Co(1)-O(1) bond lengths are 2.00 Å. There are twelve inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(1)-O(1) bond length is 1.23 Å. The C(1)-O(2) bond length is 1.24 Å. In the second C site, C(2) is bonded in a distorted trigonal non-coplanar geometry to one H(1), one H(2), and one O(3) atom. The C(2)-H(1) bond length is 0.99 Å. The C(2)-H(2) bond length is 0.99 Å. The C(2)-O(3) bond length is 1.44 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(4), one C(5), and one O(3) atom. The C(3)-C(4) bond length is 1.38 Å. The C(3)-C(5) bond length is 1.41 Å. The C(3)-O(3) bond length is 1.39 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(8), and one S(1) atom. The C(4)-C(8) bond length is 1.41 Å. The C(4)-S(1) bond length is 1.76 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(3), one C(6), and one S(1) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-S(1) bond length is 1.76 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(5), one C(7), and one H(3) atom. The C(6)-C(7) bond length is 1.40 Å. The C(6)-H(3) bond length is 0.95 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(6), one C(8), and one C(9) atom. The C(7)-C(8) bond length is 1.39 Å. The C(7)-C(9) bond length is 1.53 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(4), one C(7), and one H(4) atom. The C(8)-H(4) bond length is 0.95 Å. In the ninth C site, C(9) is bonded in a tetrahedral geometry to one C(10), one C(11), one C(12), and one C(7) atom. The C(9)-C(10) bond length is 1.47 Å. The C(9)-C(11) bond length is 1.59 Å. The C(9)-C(12) bond length is 1.53 Å. In the tenth C site, C(10) is bonded in a trigonal non-coplanar geometry to one C(9); one H(5); one H(6,12); and one H(7,11,13) atom. The C(10)-H(5) bond length is 0.98 Å. The C(10)-H(6,12) bond length is 0.98 Å. The C(10)-H(7,11,13) bond length is 0.98 Å. In the eleventh C site, C(11) is bonded in a trigonal non-coplanar geometry to one C(9); one H(8); and two equivalent H(9,10) atoms. The C(11)-H(8) bond length is 0.98 Å. Both C(11)-H(9,10) bond lengths are 0.98 Å. In the twelfth C site, C(12) is bonded in a trigonal non-coplanar geometry to one C(9); one H(6,12); and two equivalent H(7,11,13) atoms. The C(12)-H(6,12) bond length is 0.98 Å. Both C(12)-H(7,11,13) bond lengths are 0.98 Å. There are nine inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(6) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(8) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(10) atom. In the sixth H site, H(6,12) is bonded in a single-bond geometry to one C(10) atom. In the seventh H site, H(7,11,13) is bonded in a single-bond geometry to one C(10) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(11) atom. In the ninth H site, H(9,10) is bonded in a single-bond geometry to one C(11) atom. S(1) is bonded in a water-like geometry to one C(4) and one C(5) atom. There are three inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 150 degrees geometry to one Co(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one K(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted water-like geometry to one K(1), one C(2), and one C(3) atom. Linkers: 12 CC(C)(C)c1cc2c(OCC([O])=O)c(c1)Sc1cc(C(C)(C)C)cc(c1OCC([O])=O)Sc1cc(C(C)(C)C)cc(c1OCC([O])=O)Sc1cc(C(C)(C)C)cc(c1OCC([O])=O)S2. Metal clusters: 24 [K] ,16 [Co]. The MOF has largest included sphere 5.97 A, density 1.09 g/cm3, surface area 4184.39 m2/g, accessible volume 0.39 cm3/g