KVC9H13(NO)5 crystallizes in the triclinic P-1 space group. K(1) is bonded in a 4-coordinate geometry to one O(2), one O(5), and two equivalent O(3) atoms. The K(1)-O(2) bond length is 2.77 Å. The K(1)-O(5) bond length is 2.71 Å. There is one shorter (2.70 Å) and one longer (2.72 Å) K(1)-O(3) bond length. V(1) is bonded in a 5-coordinate geometry to one N(1), one N(3), one O(1), one O(3), and one O(4) atom. The V(1)-N(1) bond length is 1.96 Å. The V(1)-N(3) bond length is 2.22 Å. The V(1)-O(1) bond length is 1.90 Å. The V(1)-O(3) bond length is 1.66 Å. The V(1)-O(4) bond length is 1.67 Å. There are nine inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one N(1), one N(2), and one N(4) atom. The C(1)-N(1) bond length is 1.34 Å. The C(1)-N(2) bond length is 1.36 Å. The C(1)-N(4) bond length is 1.34 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(3), one C(6), and one O(1) atom. The C(2)-C(3) bond length is 1.42 Å. The C(2)-C(6) bond length is 1.42 Å. The C(2)-O(1) bond length is 1.33 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(2), one C(9), and one N(5) atom. The C(3)-C(9) bond length is 1.49 Å. The C(3)-N(5) bond length is 1.34 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(5), one N(5), and one H(5) atom. The C(4)-C(5) bond length is 1.39 Å. The C(4)-N(5) bond length is 1.35 Å. The C(4)-H(5) bond length is 1.09 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(4), one C(6), and one C(8) atom. The C(5)-C(6) bond length is 1.42 Å. The C(5)-C(8) bond length is 1.51 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(2), one C(5), and one C(7) atom. The C(6)-C(7) bond length is 1.43 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(6), one N(3), and one H(6) atom. The C(7)-N(3) bond length is 1.31 Å. The C(7)-H(6) bond length is 1.09 Å. In the eighth C site, C(8) is bonded in a distorted trigonal non-coplanar geometry to one C(5), one H(7), one H(8), and one O(2) atom. The C(8)-H(7) bond length is 1.10 Å. The C(8)-H(8) bond length is 1.10 Å. The C(8)-O(2) bond length is 1.45 Å. In the ninth C site, C(9) is bonded in a distorted trigonal non-coplanar geometry to one C(3), one H(10), one H(11), and one H(9) atom. The C(9)-H(10) bond length is 1.10 Å. The C(9)-H(11) bond length is 1.09 Å. The C(9)-H(9) bond length is 1.10 Å. There are five inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one V(1), one C(1), and one H(2) atom. The N(1)-H(2) bond length is 1.02 Å. In the second N site, N(2) is bonded in a 3-coordinate geometry to one C(1), one N(3), and one H(12) atom. The N(2)-N(3) bond length is 1.37 Å. The N(2)-H(12) bond length is 1.74 Å. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one V(1), one C(7), and one N(2) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one C(1), one H(3), and one H(4) atom. The N(4)-H(3) bond length is 1.04 Å. The N(4)-H(4) bond length is 1.02 Å. In the fifth N site, N(5) is bonded in a trigonal planar geometry to one C(3), one C(4), and one H(13) atom. The N(5)-H(13) bond length is 1.68 Å. There are thirteen inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(2) and one O(4) atom. The H(1)-O(2) bond length is 1.00 Å. The H(1)-O(4) bond length is 1.70 Å. In the second H site, H(2) is bonded in a single-bond geometry to one N(1) atom. In the third H site, H(3) is bonded in a single-bond geometry to one N(4) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one N(4) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(4) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(7) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(8) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(8) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(9) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(9) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(9) atom. In the twelfth H site, H(12) is bonded in a single-bond geometry to one N(2) and one O(5) atom. The H(12)-O(5) bond length is 1.00 Å. In the thirteenth H site, H(13) is bonded in a distorted single-bond geometry to one N(5) and one O(5) atom. The H(13)-O(5) bond length is 1.02 Å. There are five inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 150 degrees geometry to one V(1) and one C(2) atom. In the second O site, O(2) is bonded in a distorted water-like geometry to one K(1), one C(8), and one H(1) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to two equivalent K(1) and one V(1) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to one V(1) and one H(1) atom. In the fifth O site, O(5) is bonded in a water-like geometry to one K(1), one H(12), and one H(13) atom. Linkers: 2 Cc1ncc(CO)c(/C=N/[N]C(=N)N)c1[O]. Metal clusters: 2 [K] ,2 [V]. The MOF has largest included sphere 1.51 A, density 1.85 g/cm3, surface area 2976.13 m2/g, accessible volume 0.08 cm3/g