V8NiC8N4H8O13(C3H2)4 crystallizes in the tetragonal P-4n2 space group. The structure consists of eight 2,3-dimethyl-1,3-butadiene molecules inside a V8NiC8N4H8O13 framework. In the V8NiC8N4H8O13 framework, there are four inequivalent V sites. In the first V site, V(1) is bonded in a 5-coordinate geometry to one O(1), one O(2), one O(3), one O(4), and one O(5) atom. The V(1)-O(1) bond length is 1.63 Å. The V(1)-O(2) bond length is 1.94 Å. The V(1)-O(3) bond length is 1.93 Å. The V(1)-O(4) bond length is 1.93 Å. The V(1)-O(5) bond length is 1.95 Å. In the second V site, V(2) is bonded in a distorted see-saw-like geometry to one O(2), one O(3), one O(5), and one O(6) atom. The V(2)-O(2) bond length is 1.92 Å. The V(2)-O(3) bond length is 1.98 Å. The V(2)-O(5) bond length is 1.89 Å. The V(2)-O(6) bond length is 1.88 Å. In the third V site, V(3) is bonded in a distorted see-saw-like geometry to one O(3), one O(4), one O(5), and one O(6) atom. The V(3)-O(3) bond length is 1.89 Å. The V(3)-O(4) bond length is 1.93 Å. The V(3)-O(5) bond length is 1.95 Å. The V(3)-O(6) bond length is 1.85 Å. In the fourth V site, V(4) is bonded in a distorted see-saw-like geometry to one O(2), one O(4), one O(6), and one O(7) atom. The V(4)-O(2) bond length is 1.90 Å. The V(4)-O(4) bond length is 1.89 Å. The V(4)-O(6) bond length is 2.11 Å. The V(4)-O(7) bond length is 1.83 Å. Ni(1) is bonded in an octahedral geometry to two equivalent N(1), two equivalent N(2), and two equivalent O(1) atoms. Both Ni(1)-N(1) bond lengths are 2.14 Å. Both Ni(1)-N(2) bond lengths are 2.15 Å. Both Ni(1)-O(1) bond lengths are 2.04 Å. There are four inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(1) atom. The C(1)-N(2) bond length is 1.32 Å. The C(1)-H(1) bond length is 0.93 Å. In the second C site, C(5) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(4) atom. The C(5)-N(2) bond length is 1.35 Å. The C(5)-H(4) bond length is 0.93 Å. In the third C site, C(6) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(5) atom. The C(6)-N(1) bond length is 1.33 Å. The C(6)-H(5) bond length is 0.93 Å. In the fourth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(8) atom. The C(10)-N(1) bond length is 1.36 Å. The C(10)-H(8) bond length is 0.93 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Ni(1), one C(10), and one C(6) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ni(1), one C(1), and one C(5) atom. There are four 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. There are seven inequivalent O sites. In the first O site, O(1) is bonded in a linear geometry to one V(1) and one Ni(1) atom. In the second O site, O(2) is bonded in a distorted trigonal non-coplanar geometry to one V(1), one V(2), and one V(4) atom. In the third O site, O(3) is bonded in a distorted T-shaped geometry to one V(1), one V(2), and one V(3) atom. In the fourth O site, O(4) is bonded in a distorted trigonal non-coplanar geometry to one V(1), one V(3), and one V(4) atom. In the fifth O site, O(5) is bonded in a distorted T-shaped geometry to one V(1), one V(2), and one V(3) atom. In the sixth O site, O(6) is bonded in a T-shaped geometry to one V(2), one V(3), and one V(4) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to two equivalent V(4) atoms. Linkers: 8 c1cc(-c2ccncc2)ccn1. Metal clusters: 32 [V] ,4 [Ni]. The MOF has largest included sphere 5.35 A, density 1.54 g/cm3, surface area 2791.87 m2/g, accessible volume 0.31 cm3/g