VC8H3O5 crystallizes in the tetragonal P4_122 space group. There are two inequivalent V sites. In the first V site, V(1) is bonded to two equivalent O(1), two equivalent O(2), and two equivalent O(5) atoms to form corner-sharing VO6 octahedra. The corner-sharing octahedral tilt angles are 38°. Both V(1)-O(1) bond lengths are 1.92 Å. Both V(1)-O(2) bond lengths are 2.08 Å. Both V(1)-O(5) bond lengths are 1.88 Å. In the second V site, V(2) is bonded to two equivalent O(3), two equivalent O(4), and two equivalent O(6) atoms to form corner-sharing VO6 octahedra. The corner-sharing octahedral tilt angles are 62°. Both V(2)-O(3) bond lengths are 1.90 Å. Both V(2)-O(4) bond lengths are 1.98 Å. Both V(2)-O(6) bond lengths are 2.00 Å. There are eight inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.42 Å. The C(1)-O(1) bond length is 1.29 Å. The C(1)-O(2) bond length is 1.29 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(4) atom. The C(2)-C(3) bond length is 1.39 Å. The C(2)-C(4) bond length is 1.38 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(5), and one H(1) atom. The C(3)-C(5) bond length is 1.38 Å. The C(3)-H(1) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a single-bond geometry to one C(2), one C(6), and one H(2) atom. The C(4)-C(6) bond length is 1.38 Å. The C(4)-H(2) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(3), one C(7), and one C(8) atom. The C(5)-C(7) bond length is 1.38 Å. The C(5)-C(8) bond length is 1.42 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(4), one C(6), and one C(7) atom. The C(6)-C(6) bond length is 1.51 Å. The C(6)-C(7) bond length is 1.38 Å. In the seventh C site, C(7) is bonded in a single-bond geometry to one C(5), one C(6), and one H(3) atom. The C(7)-H(3) bond length is 0.93 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(3), and one O(4) atom. The C(8)-O(3) bond length is 1.29 Å. The C(8)-O(4) bond length is 1.29 Å. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. There are six inequivalent O sites. In the first O site, O(5) is bonded in a bent 150 degrees geometry to two equivalent V(1) atoms. In the second O site, O(6) is bonded in a bent 120 degrees geometry to two equivalent V(2) atoms. In the third O site, O(1) is bonded in a bent 150 degrees geometry to one V(1) and one C(1) atom. In the fourth O site, O(2) is bonded in a bent 150 degrees geometry to one V(1) and one C(1) atom. In the fifth O site, O(3) is bonded in a bent 150 degrees geometry to one V(2) and one C(8) atom. In the sixth O site, O(4) is bonded in a bent 120 degrees geometry to one V(2) and one C(8) atom. Linkers: 4 [O]C(=O)c1cc(C([O])=O)cc(-c2cc(C([O])=O)cc(C([O])=O)c2)c1. Metal clusters: 8 [V]. The MOF has largest included sphere 7.25 A, density 1.13 g/cm3, surface area 3266.42 m2/g, accessible volume 0.51 cm3/g