KVCPH3O7 crystallizes in the monoclinic C2/c space group. K(1) is bonded in a 9-coordinate geometry to one O(2), one O(3), one O(4), one O(5), one O(6), two equivalent O(1), and two equivalent O(7) atoms. The K(1)-O(2) bond length is 2.82 Å. The K(1)-O(3) bond length is 2.86 Å. The K(1)-O(4) bond length is 3.18 Å. The K(1)-O(5) bond length is 3.09 Å. The K(1)-O(6) bond length is 2.69 Å. There is one shorter (2.87 Å) and one longer (2.97 Å) K(1)-O(1) bond length. There is one shorter (2.77 Å) and one longer (2.83 Å) K(1)-O(7) bond length. V(1) 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 V(1)-O(1) bond length is 2.32 Å. The V(1)-O(2) bond length is 2.04 Å. The V(1)-O(3) bond length is 2.02 Å. The V(1)-O(4) bond length is 2.00 Å. The V(1)-O(5) bond length is 2.00 Å. The V(1)-O(6) bond length is 1.61 Å. 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 1.26 Å. The C(1)-O(2) bond length is 1.28 Å. P(1) is bonded in a distorted tetrahedral geometry to one H(1), one O(3), one O(4), and one O(5) atom. The P(1)-H(1) bond length is 1.41 Å. The P(1)-O(3) bond length is 1.54 Å. The P(1)-O(4) bond length is 1.54 Å. The P(1)-O(5) bond length is 1.55 Å. There are three inequivalent H sites. In the first H site, H(3) is bonded in a single-bond geometry to one O(7) atom. The H(3)-O(7) bond length is 0.98 Å. In the second H site, H(1) is bonded in a single-bond geometry to one P(1) atom. In the third H site, H(2) is bonded in a single-bond geometry to one O(7) atom. The H(2)-O(7) bond length is 0.99 Å. There are seven inequivalent O sites. In the first O site, O(3) is bonded in a 2-coordinate geometry to one K(1), one V(1), and one P(1) atom. In the second O site, O(4) is bonded in a distorted bent 120 degrees geometry to one K(1), one V(1), and one P(1) atom. In the third O site, O(5) is bonded in a distorted bent 120 degrees geometry to one K(1), one V(1), and one P(1) atom. In the fourth O site, O(6) is bonded in a distorted single-bond geometry to one K(1) and one V(1) atom. In the fifth O site, O(2) is bonded in a 3-coordinate geometry to one K(1), one V(1), and one C(1) atom. In the sixth O site, O(7) is bonded in a water-like geometry to two equivalent K(1), one H(2), and one H(3) atom. In the seventh O site, O(1) is bonded in a distorted single-bond geometry to two equivalent K(1), one V(1), and one C(1) atom. Linkers: 2 [O]C(=O)C([O])=O. Metal clusters: 4 [K] ,4 [V]. The MOF has largest included sphere 2.04 A, density 2.41 g/cm3, surface area 1458.59 m2/g, accessible volume 0.03 cm3/g