KCoC8H14(NO5)2 crystallizes in the monoclinic P2_1/c space group. K(1) is bonded in a distorted body-centered cubic geometry to two equivalent O(2), two equivalent O(5), and four equivalent O(4) atoms. Both K(1)-O(2) bond lengths are 2.76 Å. Both K(1)-O(5) bond lengths are 3.13 Å. There are two shorter (2.95 Å) and two longer (3.17 Å) K(1)-O(4) bond lengths. Co(1) is bonded in an octahedral geometry to two equivalent N(1), two equivalent O(1), and two equivalent O(3) atoms. Both Co(1)-N(1) bond lengths are 1.94 Å. Both Co(1)-O(1) bond lengths are 1.89 Å. Both Co(1)-O(3) bond lengths are 1.91 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 1.31 Å. The C(1)-O(2) bond length is 1.25 Å. In the second C site, C(2) is bonded in a distorted trigonal non-coplanar geometry to one N(1), one H(2), and one H(3) atom. The C(2)-N(1) bond length is 1.48 Å. The C(2)-H(2) bond length is 1.10 Å. The C(2)-H(3) bond length is 1.10 Å. In the third C site, C(3) is bonded in a distorted trigonal non-coplanar geometry to one N(1), one H(5), and one H(6) atom. The C(3)-N(1) bond length is 1.48 Å. The C(3)-H(5) bond length is 1.09 Å. The C(3)-H(6) bond length is 1.10 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(3) and one O(4) atom. The C(4)-O(3) bond length is 1.31 Å. The C(4)-O(4) bond length is 1.24 Å. N(1) is bonded to one Co(1), one C(2), one C(3), and one H(1) atom to form distorted corner-sharing NCoHC2 tetrahedra. The N(1)-H(1) bond length is 1.03 Å. There are seven inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one N(1) 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(2) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(5) atom. The H(4)-O(5) bond length is 0.98 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(3) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(3) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one O(5) atom. The H(7)-O(5) bond length is 0.99 Å. There are five inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Co(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one K(1) and one C(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Co(1) and one C(4) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to two equivalent K(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a water-like geometry to one K(1), one H(4), and one H(7) atom. Linkers: 4 [O]C(=O)CNCC([O])=O. Metal clusters: 2 [K] ,2 [Co]. The MOF has largest included sphere 1.58 A, density 1.93 g/cm3, surface area 2581.34 m2/g, accessible volume 0.09 cm3/g