NiC6H4(NO2)2(C4H3)2(CH)4 crystallizes in the monoclinic C2/c space group. The structure is zero-dimensional and consists of thirty-two 02329_fluka molecules, sixteen isobutylene molecules, and eight NiC6H4(NO2)2 clusters. In each NiC6H4(NO2)2 cluster, Ni(1) is bonded in a rectangular see-saw-like geometry to one N(1), one N(2), one O(1), and one O(2) atom. The Ni(1)-N(1) bond length is 2.06 Å. The Ni(1)-N(2) bond length is 2.10 Å. The Ni(1)-O(1) bond length is 2.08 Å. The Ni(1)-O(2) bond length is 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 O(2) and one O(4) atom. The C(10)-O(2) bond length is 1.26 Å. The C(10)-O(4) bond length is 1.25 Å. In the second C site, C(11) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(3) atom. The C(11)-O(1) bond length is 1.26 Å. The C(11)-O(3) bond length is 1.27 Å. In the third C site, C(12) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(9) atom. The C(12)-N(1) bond length is 1.34 Å. The C(12)-H(9) bond length is 0.93 Å. In the fourth C site, C(14) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(11) atom. The C(14)-N(2) bond length is 1.32 Å. The C(14)-H(11) bond length is 0.93 Å. In the fifth C site, C(18) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(14) atom. The C(18)-N(2) bond length is 1.32 Å. The C(18)-H(14) bond length is 0.93 Å. In the sixth C site, C(2) is bonded in a distorted bent 120 degrees geometry to 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 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(12), and one C(2) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ni(1), one C(14), and one C(18) atom. There are four inequivalent H sites. In the first H site, H(2) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(9) is bonded in a single-bond geometry to one C(12) atom. In the third H site, H(11) is bonded in a single-bond geometry to one C(14) atom. In the fourth H site, H(14) is bonded in a single-bond geometry to one C(18) atom. There are four inequivalent O sites. In the first O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(10) atom. In the second O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(11) atom. In the third O site, O(3) is bonded in a single-bond geometry to one C(11) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(10) atom. Linkers: 8 C(=C/c1ccncc1)\c1ccncc1 ,8 [O]C(=O)/C=C/C=C/C([O])=O ,4 [c]1cc(/C=C/c2ccncc2)ccn1. Metal clusters: 8 O=[C]O[Ni]O[C]=O. The MOF has largest included sphere 6.68 A, density 1.12 g/cm3, surface area 5139.01 m2/g, accessible volume 0.39 cm3/g