V2CoC6N3H6O4(C3H2)3 crystallizes in the monoclinic C2/c space group. The structure consists of twelve 2,3-dimethyl-1,3-butadiene molecules inside a V2CoC6N3H6O4 framework. In the V2CoC6N3H6O4 framework, there are two inequivalent V sites. In the first V site, V(1) is bonded in a trigonal non-coplanar geometry to one O(1), one O(2), and one O(3) atom. The V(1)-O(1) bond length is 1.67 Å. The V(1)-O(2) bond length is 1.78 Å. The V(1)-O(3) bond length is 1.80 Å. In the second V site, V(2) is bonded in a trigonal non-coplanar geometry to one O(2), one O(3), and one O(4) atom. The V(2)-O(2) bond length is 1.80 Å. The V(2)-O(3) bond length is 1.80 Å. The V(2)-O(4) bond length is 1.67 Å. There are two inequivalent Co sites. In the first Co site, Co(1) is bonded in an octahedral geometry to two equivalent N(1), two equivalent N(2), and two equivalent O(1) atoms. Both Co(1)-N(1) bond lengths are 2.19 Å. Both Co(1)-N(2) bond lengths are 2.26 Å. Both Co(1)-O(1) bond lengths are 2.02 Å. In the second Co site, Co(2) is bonded in a square co-planar geometry to two equivalent N(3) and two equivalent O(4) atoms. Both Co(2)-N(3) bond lengths are 2.14 Å. Both Co(2)-O(4) bond lengths are 2.04 Å. There are six inequivalent C sites. In the first C site, C(10) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(8) atom. The C(10)-N(2) bond length is 1.34 Å. The C(10)-H(8) bond length is 0.93 Å. In the second C site, C(11) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(9) atom. The C(11)-N(3) bond length is 1.34 Å. The C(11)-H(9) bond length is 0.93 Å. In the third C site, C(15) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(12) atom. The C(15)-N(3) bond length is 1.33 Å. The C(15)-H(12) bond length is 0.93 Å. In the fourth C site, C(1) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(1) atom. The C(1)-N(1) bond length is 1.35 Å. The C(1)-H(1) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(4) atom. The C(5)-N(1) bond length is 1.34 Å. The C(5)-H(4) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(5) atom. The C(6)-N(2) bond length is 1.34 Å. The C(6)-H(5) bond length is 0.93 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Co(1), one C(1), and one C(5) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Co(1), one C(10), and one C(6) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Co(2), one C(11), and one C(15) atom. There are six 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(4) is bonded in a single-bond geometry to one C(5) atom. In the third H site, H(5) is bonded in a single-bond geometry to one C(6) atom. In the fourth H site, H(8) is bonded in a single-bond geometry to one C(10) atom. In the fifth H site, H(9) is bonded in a single-bond geometry to one C(11) atom. In the sixth H site, H(12) is bonded in a single-bond geometry to one C(15) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a bent 150 degrees geometry to one V(1) and one Co(1) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one V(1) and one V(2) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one V(1) and one V(2) atom. In the fourth O site, O(4) is bonded in a bent 150 degrees geometry to one V(2) and one Co(2) atom. Linkers: 5 c1cc(-c2ccncc2)ccn1. Metal clusters: 8 [V] ,4 [Co]. The MOF has largest included sphere 4.62 A, density 1.59 g/cm3, surface area 3855.18 m2/g, accessible volume 0.19 cm3/g