C2H2CuNO6V2 crystallizes in the triclinic P-1 space group. There are two inequivalent V sites. In the first V site, V(1) is bonded to one O(1), one O(4), one O(5), and one O(6) atom to form VO4 tetrahedra that share corners with two equivalent Cu(1)NO4 square pyramids and corners with two equivalent V(2)O4 tetrahedra. The V(1)-O(1) bond length is 1.63 Å. The V(1)-O(4) bond length is 1.69 Å. The V(1)-O(5) bond length is 1.81 Å. The V(1)-O(6) bond length is 1.79 Å. In the second V site, V(2) is bonded to one O(2), one O(3), one O(5), and one O(6) atom to form VO4 tetrahedra that share corners with two equivalent Cu(1)NO4 square pyramids and corners with two equivalent V(1)O4 tetrahedra. The V(2)-O(2) bond length is 1.68 Å. The V(2)-O(3) bond length is 1.68 Å. The V(2)-O(5) bond length is 1.79 Å. The V(2)-O(6) bond length is 1.78 Å. Cu(1) is bonded to one N(1), one O(1), one O(2), one O(3), and one O(4) atom to form distorted CuNO4 square pyramids that share corners with two equivalent V(1)O4 tetrahedra and corners with two equivalent V(2)O4 tetrahedra. The Cu(1)-N(1) bond length is 2.00 Å. The Cu(1)-O(1) bond length is 2.28 Å. The Cu(1)-O(2) bond length is 1.95 Å. The Cu(1)-O(3) bond length is 1.96 Å. The Cu(1)-O(4) bond length is 1.91 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one N(1), and one H(1) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-N(1) bond length is 1.34 Å. The C(1)-H(1) bond length is 1.09 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1), one N(1), and one H(2) atom. The C(2)-N(1) bond length is 1.34 Å. The C(2)-H(2) bond length is 1.09 Å. N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(2) atom. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(2) atom. There are six inequivalent O sites. In the first O site, O(1) is bonded in a bent 150 degrees geometry to one V(1) and one Cu(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one V(2) and one Cu(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one V(2) and one Cu(1) atom. In the fourth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one V(1) and one Cu(1) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one V(1) and one V(2) atom. In the sixth O site, O(6) is bonded in a bent 150 degrees geometry to one V(1) and one V(2) atom. Linkers: 1 c1cnccn1. Metal clusters: 4 [V] ,2 [Cu]. The MOF has largest included sphere 1.55 A, density 2.95 g/cm3, surface area 2105.67 m2/g, accessible volume 0.03 cm3/g