NiC14H8(NO)4(CH)2 crystallizes in the tetragonal P4_32_12 space group. The structure consists of eight 02329_fluka molecules inside a NiC14H8(NO)4 framework. In the NiC14H8(NO)4 framework, Ni(1) is bonded in a distorted octahedral geometry to two equivalent N(1), two equivalent O(1), and two equivalent O(2) atoms. Both Ni(1)-N(1) bond lengths are 2.01 Å. Both Ni(1)-O(1) bond lengths are 2.25 Å. Both Ni(1)-O(2) bond lengths are 2.07 Å. There are seven inequivalent C sites. In the first C site, C(8) is bonded in a trigonal planar geometry to one N(1), one N(2), and one H(1) atom. The C(8)-N(1) bond length is 1.33 Å. The C(8)-N(2) bond length is 1.35 Å. The C(8)-H(1) bond length is 1.08 Å. In the second 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)-C(2) bond length is 1.49 Å. The C(1)-O(1) bond length is 1.28 Å. The C(1)-O(2) bond length is 1.29 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2) and one H(4) atom. The C(3)-C(2) bond length is 1.42 Å. The C(3)-H(4) bond length is 1.09 Å. In the fourth C site, C(5) is bonded in a distorted single-bond geometry to one C(6) and one N(1) atom. The C(5)-C(6) bond length is 1.42 Å. The C(5)-N(1) bond length is 1.39 Å. In the fifth C site, C(7) is bonded in a distorted single-bond geometry to one C(2), one C(6), and one H(3) atom. The C(7)-C(2) bond length is 1.40 Å. The C(7)-C(6) bond length is 1.39 Å. The C(7)-H(3) bond length is 1.09 Å. In the sixth C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(7) atom. In the seventh C site, C(6) is bonded in a distorted single-bond geometry to one C(5), one C(7), and one N(2) atom. The C(6)-N(2) bond length is 1.38 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(5), and one C(8) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one C(6), one C(8), and one H(2) atom. The N(2)-H(2) bond length is 1.02 Å. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(8) atom. In the second H site, H(2) is bonded in a single-bond geometry to one N(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(3) atom. There are two inequivalent O sites. In the first O site, O(2) is bonded in an L-shaped geometry to one Ni(1) and one C(1) atom. In the second O site, O(1) is bonded in a distorted L-shaped geometry to one Ni(1) and one C(1) atom. Linkers: 1 [O]C(=O)c1ccc2c(c1)N[CH]N2[Ni]12(N3[CH]Nc4cc(C([O])=O)ccc43)(O[C](c3ccc4nc[nH]c4c3)O1)O[C](c1ccc3nc[nH]c3c1)O2 ,4 [O]C(=O)c1ccc2nc[nH]c2c1. Metal clusters: 3 [C]1O[Ni]2(O1)O[C]O2. The MOF has largest included sphere 4.57 A, density 1.33 g/cm3, surface area 4075.24 m2/g, accessible volume 0.25 cm3/g