NiC9H4(NO2)2 crystallizes in the monoclinic C2/c space group. Ni(1) is bonded in a rectangular see-saw-like geometry to one N(1), one N(2), one O(1), and one O(3) atom. The Ni(1)-N(1) bond length is 2.12 Å. The Ni(1)-N(2) bond length is 2.12 Å. The Ni(1)-O(1) bond length is 2.04 Å. The Ni(1)-O(3) bond length is 2.07 Å. There are eleven inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(8), one N(1), and one H(1) atom. The C(1)-C(8) bond length is 1.39 Å. The C(1)-N(1) bond length is 1.33 Å. The C(1)-H(1) bond length is 0.93 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(10), one N(2), and one H(2) atom. The C(2)-C(10) bond length is 1.40 Å. The C(2)-N(2) bond length is 1.33 Å. The C(2)-H(2) bond length is 0.93 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(4), one C(5), and one C(6) atom. The C(3)-C(4) bond length is 1.41 Å. The C(3)-C(5) bond length is 1.40 Å. The C(3)-C(6) bond length is 1.49 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(5), and one C(7) atom. The C(4)-C(5) bond length is 1.38 Å. The C(4)-C(7) bond length is 1.51 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(3), one C(4), and one H(3) atom. The C(5)-H(3) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(1), and one O(2) atom. The C(6)-O(1) bond length is 1.26 Å. The C(6)-O(2) bond length is 1.25 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(7)-O(3) bond length is 1.27 Å. The C(7)-O(4) bond length is 1.22 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(10) and two equivalent C(1) atoms. The C(8)-C(10) bond length is 1.47 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to two equivalent N(1) and one H(4) atom. Both C(9)-N(1) bond lengths are 1.32 Å. The C(9)-H(4) bond length is 0.93 Å. In the tenth C site, C(10) is bonded in a trigonal planar geometry to one C(8) and two equivalent C(2) atoms. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to two equivalent N(2) and one H(5) atom. Both C(11)-N(2) bond lengths are 1.33 Å. The C(11)-H(5) 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(1), and one C(9) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ni(1), one C(11), and one C(2) atom. There are five 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(5) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(9) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(11) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(6) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(6) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(7) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(7) atom. Linkers: 3 [O]C(=O)c1cc(C([O])=O)c(C([O])=O)cc1C([O])=O ,2 c1ncc(-c2cncnc2)cn1. Metal clusters: 4 O=[C]O[Ni]O[C]=O. The MOF has largest included sphere 4.16 A, density 1.33 g/cm3, surface area 3955.60 m2/g, accessible volume 0.36 cm3/g