K3CH(NO)6 crystallizes in the monoclinic C2/c space group. There are three inequivalent K sites. In the first K site, K(1) is bonded in a 8-coordinate geometry to one N(2), one N(4), one O(1), one O(5), two equivalent O(2), and two equivalent O(6) atoms. The K(1)-N(2) bond length is 2.91 Å. The K(1)-N(4) bond length is 2.97 Å. The K(1)-O(1) bond length is 2.81 Å. The K(1)-O(5) bond length is 2.63 Å. Both K(1)-O(2) bond lengths are 2.76 Å. There is one shorter (2.89 Å) and one longer (2.91 Å) K(1)-O(6) bond length. In the second K site, K(2) is bonded in a 6-coordinate geometry to one O(1), one O(2), one O(3), one O(4), one O(5), and one O(6) atom. The K(2)-O(1) bond length is 2.84 Å. The K(2)-O(2) bond length is 2.87 Å. The K(2)-O(3) bond length is 2.78 Å. The K(2)-O(4) bond length is 2.83 Å. The K(2)-O(5) bond length is 2.73 Å. The K(2)-O(6) bond length is 2.83 Å. In the third K site, K(3) is bonded in a 6-coordinate geometry to one O(1), one O(5), two equivalent O(3), and two equivalent O(4) atoms. The K(3)-O(1) bond length is 2.62 Å. The K(3)-O(5) bond length is 2.76 Å. There is one shorter (2.73 Å) and one longer (2.91 Å) K(3)-O(3) bond length. There is one shorter (2.78 Å) and one longer (2.82 Å) K(3)-O(4) bond length. C(1) is bonded in a tetrahedral geometry to one N(1), one N(3), one N(5), and one H(1) atom. The C(1)-N(1) bond length is 1.46 Å. The C(1)-N(3) bond length is 1.47 Å. The C(1)-N(5) bond length is 1.47 Å. The C(1)-H(1) bond length is 1.10 Å. There are six inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one C(1), one N(2), and one O(1) atom. The N(1)-N(2) bond length is 1.32 Å. The N(1)-O(1) bond length is 1.30 Å. In the second N site, N(2) is bonded in a 1-coordinate geometry to one K(1), one N(1), and one O(2) atom. The N(2)-O(2) bond length is 1.29 Å. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one C(1), one N(4), and one O(3) atom. The N(3)-N(4) bond length is 1.32 Å. The N(3)-O(3) bond length is 1.30 Å. In the fourth N site, N(4) is bonded in a 1-coordinate geometry to one K(1), one N(3), and one O(4) atom. The N(4)-O(4) bond length is 1.29 Å. In the fifth N site, N(5) is bonded in a distorted bent 120 degrees geometry to one C(1) and one O(5) atom. The N(5)-O(5) bond length is 1.31 Å. In the sixth N site, N(6) is bonded in a distorted single-bond geometry to one O(6) atom. The N(6)-O(6) bond length is 1.30 Å. H(1) is bonded in a single-bond geometry to one C(1) atom. There are six inequivalent O sites. In the first O site, O(3) is bonded in a 4-coordinate geometry to one K(2), two equivalent K(3), and one N(3) atom. In the second O site, O(4) is bonded in a 4-coordinate geometry to one K(2), two equivalent K(3), and one N(4) atom. In the third O site, O(5) is bonded in a 4-coordinate geometry to one K(1), one K(2), one K(3), and one N(5) atom. In the fourth O site, O(6) is bonded in a distorted single-bond geometry to one K(2), two equivalent K(1), and one N(6) atom. In the fifth O site, O(2) is bonded in a distorted single-bond geometry to one K(2), two equivalent K(1), and one N(2) atom. In the sixth O site, O(1) is bonded in a 4-coordinate geometry to one K(1), one K(2), one K(3), and one N(1) atom. Linkers: 4 [O][N]N([O])C(N([O])[N][O])N([O])[N][O]. Metal clusters: 12 [K]. The MOF has largest included sphere 1.22 A, density 2.16 g/cm3, surface area 483.92 m2/g, accessible volume 0.01 cm3/g