CuC6H6(NO)2 crystallizes in the tetragonal I4_1md space group. Cu(1) is bonded in a distorted rectangular see-saw-like geometry to two equivalent N(1) and two equivalent O(1) atoms. Both Cu(1)-N(1) bond lengths are 1.97 Å. Both Cu(1)-O(1) bond lengths are 2.01 Å. There are four inequivalent C sites. In the first C site, C(3) is bonded in a trigonal planar geometry to one C(4) and two equivalent C(1) atoms. The C(3)-C(4) bond length is 1.43 Å. Both C(3)-C(1) bond lengths are 1.40 Å. In the second C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(3) and two equivalent O(1) atoms. Both C(4)-O(1) bond lengths are 1.27 Å. In the third C site, C(1) is bonded in a 3-coordinate geometry to one C(2), one C(3), and one N(1) atom. The C(1)-C(2) bond length is 1.50 Å. The C(1)-N(1) bond length is 1.33 Å. In the fourth C site, C(2) is bonded in a trigonal non-coplanar geometry to one C(1) and three equivalent H(1,2,3) atoms. All C(2)-H(1,2,3) bond lengths are 0.97 Å. N(1) is bonded in a 2-coordinate geometry to one Cu(1) and one C(1) atom. H(1,2,3) is bonded in a single-bond geometry to one C(2) atom. O(1) is bonded in an L-shaped geometry to one Cu(1) and one C(4) atom. Linkers: 3 CC1=N[N]C(C)=C1C([O])=O ,1 CC1=NN=C(C)[C]1C([O])=O. Metal clusters: 2 [C]1O[Cu]2(N=N[Cu]3(N=N2)O[C]O3)O1. The MOF has largest included sphere 10.34 A, density 0.63 g/cm3, surface area 3913.72 m2/g, accessible volume 1.20 cm3/g