Cu2C4N3H4I(CH2)2(CH3)2 crystallizes in the tetragonal I4_1/a space group. The structure consists of thirty-two 02329_fluka molecules and thirty-two 02329_fluka molecules inside a Cu2C4N3H4I framework. In the Cu2C4N3H4I framework, there are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a distorted single-bond geometry to one N(2) and three equivalent I(1) atoms. The Cu(1)-N(2) bond length is 1.98 Å. There are a spread of Cu(1)-I(1) bond distances ranging from 2.56-3.14 Å. In the second Cu site, Cu(2) is bonded in a distorted bent 150 degrees geometry to one N(1), one N(3), and two equivalent I(1) atoms. The Cu(2)-N(1) bond length is 1.89 Å. The Cu(2)-N(3) bond length is 1.89 Å. There is one shorter (3.08 Å) and one longer (3.18 Å) Cu(2)-I(1) bond length. There are four inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one N(1), and one N(3) atom. The C(1)-C(2) bond length is 1.49 Å. The C(1)-N(1) bond length is 1.33 Å. The C(1)-N(3) bond length is 1.36 Å. In the second C site, C(5) is bonded in a distorted trigonal planar geometry to one C(6), one N(2), and one N(3) atom. The C(5)-C(6) bond length is 1.49 Å. The C(5)-N(2) bond length is 1.34 Å. The C(5)-N(3) bond length is 1.37 Å. In the third C site, C(2) is bonded in a distorted water-like geometry to one C(1), one H(1), and one H(2) atom. The C(2)-H(1) bond length is 1.10 Å. The C(2)-H(2) bond length is 1.10 Å. In the fourth C site, C(6) is bonded in a distorted water-like geometry to one C(5), one H(8), and one H(9) atom. The C(6)-H(8) bond length is 1.10 Å. The C(6)-H(9) bond length is 1.10 Å. There are three inequivalent N sites. In the first N site, N(2) is bonded in a 3-coordinate geometry to one Cu(1), one C(5), and one N(1) atom. The N(2)-N(1) bond length is 1.38 Å. In the second N site, N(3) is bonded in a trigonal planar geometry to one Cu(2), one C(1), and one C(5) atom. In the third N site, N(1) is bonded in a distorted trigonal planar geometry to one Cu(2), one C(1), and one N(2) atom. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(9) is bonded in a single-bond geometry to one C(6) atom. In the third H site, H(2) is bonded in a single-bond geometry to one C(2) atom. In the fourth H site, H(8) is bonded in a single-bond geometry to one C(6) atom. I(1) is bonded in a 5-coordinate geometry to two equivalent Cu(2) and three equivalent Cu(1) atoms. Linkers: 1 CCCC1=[N]=C(N=N1)CCC ,7 CCCC1=NN=C(CCC)[N]1. Metal clusters: 1 [Cu]/N=N\[Cu]123(I)[Cu]N=N[Cu]14(I)[Cu]21(I)N=N[Cu][Cu]413(I)/N=N\[Cu] ,1 [Cu]/N=N\[Cu]12(I)[Cu]3(I)(/N=N\[Cu])[Cu]1(I)(/N=N\[Cu])[Cu]23(I)/N=N\[Cu]. The MOF has largest included sphere 3.38 A, density 2.05 g/cm3, surface area 3293.76 m2/g, accessible volume 0.11 cm3/g