NiC10H6(NO2)2(C4H5)2 crystallizes in the cubic F4_132 space group. The structure consists of ninety-six isobutylene molecules inside a NiC10H6(NO2)2 framework. In each NiC10H6(NO2)2 framework, Ni(1) is bonded in a rectangular see-saw-like geometry to two equivalent N(1) and two equivalent O(1) atoms. Both Ni(1)-N(1) bond lengths are 2.08 Å. Both Ni(1)-O(1) bond lengths are 2.07 Å. There are five inequivalent C sites. In the first C site, C(2) is bonded in a distorted trigonal planar geometry to one C(1) and two equivalent C(3) atoms. The C(2)-C(1) bond length is 1.51 Å. Both C(2)-C(3) bond lengths are 1.39 Å. In the second C site, C(3) is bonded in a single-bond geometry to two equivalent C(2) and one H(1) atom. The C(3)-H(1) bond length is 0.93 Å. In the third C site, C(4) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(2) atom. The C(4)-N(1) bond length is 1.34 Å. The C(4)-H(2) bond length is 0.93 Å. In the fourth 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)-O(1) bond length is 1.25 Å. The C(1)-O(2) bond length is 1.26 Å. In the fifth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(8) atom. The C(9)-N(1) bond length is 1.33 Å. The C(9)-H(8) bond length is 0.93 Å. N(1) is bonded in a trigonal planar geometry to one Ni(1), one C(4), and one C(9) atom. 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(8) is bonded in a single-bond geometry to one C(9) atom. There are two inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(1) atom. Linkers: 8 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 12 [Ni]. The MOF has largest included sphere 9.78 A, density 0.91 g/cm3, surface area 5293.73 m2/g, accessible volume 0.69 cm3/g