KCo3(C4O9)2(CH2)4 crystallizes in the tetragonal I-42d space group. The structure consists of thirty-two 02329_fluka molecules inside a KCo3(C4O9)2 framework. In the KCo3(C4O9)2 framework, K(1) is bonded in a 10-coordinate geometry to two equivalent O(1), two equivalent O(4), two equivalent O(6), two equivalent O(8), and two equivalent O(9) atoms. Both K(1)-O(1) bond lengths are 2.74 Å. Both K(1)-O(4) bond lengths are 2.70 Å. Both K(1)-O(6) bond lengths are 3.01 Å. Both K(1)-O(8) bond lengths are 2.87 Å. Both K(1)-O(9) bond lengths are 2.82 Å. There are two inequivalent Co sites. In the first Co site, Co(1) is bonded to one O(1), one O(4), one O(6), and three equivalent O(3) atoms to form edge-sharing CoO6 octahedra. The Co(1)-O(1) bond length is 2.15 Å. The Co(1)-O(4) bond length is 2.06 Å. The Co(1)-O(6) bond length is 2.06 Å. There are a spread of Co(1)-O(3) bond distances ranging from 2.06-2.18 Å. In the second Co site, Co(2) is bonded in a distorted tetrahedral geometry to two equivalent O(2) and two equivalent O(7) atoms. Both Co(2)-O(2) bond lengths are 1.97 Å. Both Co(2)-O(7) bond lengths are 1.99 Å. There are four 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 1.27 Å. The C(1)-O(2) bond length is 1.25 Å. In the second C site, C(3) is bonded in a distorted single-bond geometry to one O(3) atom. The C(3)-O(3) bond length is 1.41 Å. In the third C site, C(5) is bonded in a distorted bent 120 degrees geometry to one O(6) and one O(7) atom. The C(5)-O(6) bond length is 1.25 Å. The C(5)-O(7) bond length is 1.27 Å. In the fourth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one O(4) and one O(5) atom. The C(6)-O(4) bond length is 1.26 Å. The C(6)-O(5) bond length is 1.22 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one K(1), one Co(1), and one C(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Co(2) and one C(1) atom. In the third O site, O(3) is bonded in a 4-coordinate geometry to three equivalent Co(1) and one C(3) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one K(1), one Co(1), and one C(6) atom. In the fifth O site, O(5) is bonded in a single-bond geometry to one C(6) atom. In the sixth O site, O(6) is bonded in a distorted bent 120 degrees geometry to one K(1), one Co(1), and one C(5) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Co(2) and one C(5) atom. In the eighth O site, O(8) is bonded in a distorted L-shaped geometry to one K(1) and one O(9) atom. The O(8)-O(9) bond length is 0.86 Å. In the ninth O site, O(9) is bonded in an L-shaped geometry to one K(1) and one O(8) atom. Linkers: 16 [O]C(=O)CC([O])(CC([O])=O)C([O])=O. Metal clusters: 8 [K] ,24 [Co]. The MOF has largest included sphere 4.51 A, density 1.75 g/cm3, surface area 2324.98 m2/g, accessible volume 0.20 cm3/g