NiC8H8(NO)4 crystallizes in the monoclinic C2/c space group. Ni(1) is bonded in an 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 2.10 Å. Both Ni(1)-O(2) bond lengths are 2.10 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 C(2), one N(1), and one H(1) atom. The C(1)-C(2) bond length is 1.38 Å. The C(1)-N(1) bond length is 1.38 Å. The C(1)-H(1) bond length is 1.08 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(1), one N(2), and one H(2) atom. The C(2)-N(2) bond length is 1.38 Å. The C(2)-H(2) bond length is 1.08 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(3)-O(1) bond length is 1.26 Å. The C(3)-O(2) bond length is 1.27 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one N(1), one N(2), and one H(3) atom. The C(4)-N(1) bond length is 1.33 Å. The C(4)-N(2) bond length is 1.35 Å. The C(4)-H(3) bond length is 1.08 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(1), and one C(4) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one C(2), one C(4), and one H(4) atom. The N(2)-H(4) bond length is 1.04 Å. 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(2) is bonded in a single-bond geometry to one C(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(4) atom. In the fourth H site, H(4) is bonded in a distorted single-bond geometry to one N(2) and one O(2) atom. The H(4)-O(2) bond length is 1.72 Å. There are two inequivalent O sites. In the first O site, O(1) is bonded in a distorted water-like geometry to one Ni(1) and one C(3) atom. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to one Ni(1), one C(3), and one H(4) atom. Linkers: 1 [O]C(=O)C([O])=O. Metal clusters: 2 [Ni]. The MOF has largest included sphere 2.53 A, density 1.58 g/cm3, surface area 4095.28 m2/g, accessible volume 0.17 cm3/g