NiC14H8(NO)4 crystallizes in the orthorhombic Cmmm space group. Ni(1,2) is bonded in an octahedral geometry to two equivalent N(1,2) and four equivalent O(1,2) atoms. Both Ni(1,2)-N(1,2) bond lengths are 2.03 Å. All Ni(1,2)-O(1,2) bond lengths are 2.06 Å. There are five inequivalent C sites. In the first C site, C(5,6) is bonded in a distorted bent 120 degrees geometry to two equivalent O(1,2) atoms. Both C(5,6)-O(1,2) bond lengths are 1.27 Å. In the second C site, C(7,8,9) is bonded in a distorted bent 120 degrees geometry to one C(10,11,12); one N(1,2); and one H(1,2,3) atom. The C(7,8,9)-C(10,11,12) bond length is 1.39 Å. The C(7,8,9)-N(1,2) bond length is 1.35 Å. The C(7,8,9)-H(1,2,3) bond length is 1.09 Å. In the third C site, C(10,11,12) is bonded in a distorted single-bond geometry to one C(1,2); one C(7,8,9); and one H(4,5,6) atom. The C(10,11,12)-C(1,2) bond length is 1.40 Å. The C(10,11,12)-H(4,5,6) bond length is 1.09 Å. In the fourth C site, C(1,2) is bonded in a trigonal planar geometry to one C(3,4) and two equivalent C(10,11,12) atoms. The C(1,2)-C(3,4) bond length is 1.48 Å. In the fifth C site, C(3,4) is bonded in a distorted trigonal planar geometry to one C(1,2) and two equivalent N(3,4) atoms. Both C(3,4)-N(3,4) bond lengths are 1.34 Å. There are two inequivalent N sites. In the first N site, N(1,2) is bonded in a trigonal planar geometry to one Ni(1,2) and two equivalent C(7,8,9) atoms. In the second N site, N(3,4) is bonded in a bent 120 degrees geometry to two equivalent C(3,4) atoms. There are two inequivalent H sites. In the first H site, H(1,2,3) is bonded in a single-bond geometry to one C(7,8,9) atom. In the second H site, H(4,5,6) is bonded in a single-bond geometry to one C(10,11,12) atom. O(1,2) is bonded in a water-like geometry to one Ni(1,2) and one C(5,6) atom. Linkers: 1 [O]C(=O)C([O])=O ,2 n1ccc(cc1)C1=NC(=[N]=C([N]1)c1ccncc1)c1ccncc1. Metal clusters: 3 [Ni]. The MOF has largest included sphere 20.70 A, density 0.55 g/cm3, surface area 4309.31 m2/g, accessible volume 1.51 cm3/g