Cu3C10H2(NO2)4 crystallizes in the tetragonal I4_1/acd space group. The structure consists of a Cu3C10H2(NO2)4 framework. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a distorted square co-planar geometry to one N(1), one O(2), and two equivalent O(1) atoms. The Cu(1)-N(1) bond length is 1.99 Å. The Cu(1)-O(2) bond length is 1.98 Å. There is one shorter (1.97 Å) and one longer (2.58 Å) Cu(1)-O(1) bond length. In the second Cu site, Cu(2) is bonded in a square co-planar geometry to two equivalent N(2) and two equivalent O(3) atoms. Both Cu(2)-N(2) bond lengths are 1.96 Å. Both Cu(2)-O(3) bond lengths are 1.96 Å. There are five inequivalent C sites. In the first 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 1.48 Å. The C(1)-O(1) bond length is 1.27 Å. The C(1)-O(2) bond length is 1.23 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1), one C(3), and one N(1) atom. The C(2)-C(3) bond length is 1.40 Å. The C(2)-N(1) bond length is 1.33 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(1) atom. The C(3)-C(4) bond length is 1.37 Å. The C(3)-H(1) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a 3-coordinate geometry to one C(3), one C(5), and one N(2) atom. The C(4)-C(5) bond length is 1.50 Å. The C(4)-N(2) bond length is 1.36 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(5)-O(3) bond length is 1.25 Å. The C(5)-O(4) bond length is 1.25 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a 3-coordinate geometry to one Cu(1), one C(2), and one N(2) atom. The N(1)-N(2) bond length is 1.34 Å. In the second N site, N(2) is bonded in a 3-coordinate geometry to one Cu(2), one C(4), and one N(1) atom. H(1) is bonded in a single-bond geometry to one C(3) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a 1-coordinate geometry to two equivalent Cu(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted water-like geometry to one Cu(1) and one C(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Cu(2) and one C(5) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(5) atom. Linkers: 9 [O]C(=O)[C]1C=C(C([O])=O)N=N1 ,6 [O]C(=O)C1=NN=C(C([O])=O)[CH]1 ,16 [O]C(=O)C1=CC(C([O])=O)=N[N]1. Metal clusters: 48 [Cu]. The MOF has largest included sphere 5.35 A, density 1.32 g/cm3, surface area 3388.54 m2/g, accessible volume 0.47 cm3/g