Cu3C14H6I(NO4)2 crystallizes in the tetragonal I4/mmm space group. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a 4-coordinate geometry to two equivalent N(1) and two equivalent I(1) atoms. Both Cu(1)-N(1) bond lengths are 2.05 Å. Both Cu(1)-I(1) bond lengths are 2.64 Å. In the second Cu site, Cu(2) is bonded in a distorted rectangular see-saw-like geometry to two equivalent O(1) and two equivalent O(2) atoms. Both Cu(2)-O(1) bond lengths are 1.96 Å. Both Cu(2)-O(2) bond lengths are 1.96 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 1.35 Å. The C(1)-H(1) bond length is 0.95 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(4) atom. The C(2)-C(3) bond length is 1.50 Å. The C(2)-C(4) bond length is 1.39 Å. In the third C site, C(3) is bonded in a bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(3)-O(1) bond length is 1.27 Å. The C(3)-O(2) bond length is 1.26 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to two equivalent C(2) and one H(2) atom. The C(4)-H(2) bond length is 0.95 Å. N(1) is bonded in a trigonal planar geometry to one Cu(1) and two equivalent C(1) atoms. There are two inequivalent H sites. In the first H site, H(2) is bonded in a single-bond geometry to one C(4) atom. In the second H site, H(1) is bonded in a single-bond geometry to one C(1) atom. There are two inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Cu(2) and one C(3) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Cu(2) and one C(3) atom. I(1) is bonded in a 2-coordinate geometry to two equivalent Cu(1) atoms. Linkers: 19 [O]C(=O)c1cncc(C([O])=O)c1. Metal clusters: 4 [Cu][Cu](I)I ,8 [C]1O[Cu]234O[C]O[Cu]2(O1)(O[C]O3)O[C]O4. The MOF has largest included sphere 9.87 A, density 1.20 g/cm3, surface area 2908.87 m2/g, accessible volume 0.58 cm3/g