Zr3Cu4C24H24I4(NO4)4 crystallizes in the tetragonal I4/mmm space group. There are two inequivalent Zr sites. In the first Zr site, Zr(1) is bonded in a 8-coordinate geometry to four equivalent O(2) and four equivalent O(3) atoms. All Zr(1)-O(2) bond lengths are 2.17 Å. All Zr(1)-O(3) bond lengths are 2.26 Å. In the second Zr site, Zr(2) is bonded in a 8-coordinate geometry to two equivalent O(1), two equivalent O(4), and four equivalent O(3) atoms. Both Zr(2)-O(1) bond lengths are 2.34 Å. Both Zr(2)-O(4) bond lengths are 1.95 Å. All Zr(2)-O(3) bond lengths are 2.35 Å. Cu(1) is bonded in a distorted single-bond geometry to one N(1) and three equivalent I(1) atoms. The Cu(1)-N(1) bond length is 1.99 Å. There is one shorter (2.65 Å) and two longer (2.76 Å) Cu(1)-I(1) bond lengths. There are six inequivalent C sites. In the first C site, C(2) is bonded in a distorted single-bond geometry to one C(3) and one H(4) atom. The C(2)-C(3) bond length is 1.40 Å. The C(2)-H(4) bond length is 1.09 Å. In the second C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(6) atom. The C(3)-C(4) bond length is 1.40 Å. The C(3)-C(6) bond length is 1.50 Å. In the third C site, C(4) is bonded in a distorted trigonal planar geometry to one C(3), one C(5), and one H(5) atom. The C(4)-C(5) bond length is 1.39 Å. The C(4)-H(5) bond length is 1.09 Å. In the fourth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(4), one N(1), and one H(6) atom. The C(5)-N(1) bond length is 1.35 Å. The C(5)-H(6) bond length is 1.09 Å. In the fifth C site, C(6) is bonded in a 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 1.29 Å. In the sixth C site, C(1) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(3) atom. The C(1)-N(1) bond length is 1.35 Å. The C(1)-H(3) bond length is 1.09 Å. N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(5) atom. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(3) atom. The H(1)-O(3) bond length is 0.98 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(4) atom. The H(2)-O(4) bond length is 0.96 Å. In the third H site, H(3) is bonded in a single-bond geometry to one C(1) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(2) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(4) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(5) atom. There are four inequivalent O sites. In the first O site, O(2) is bonded in a distorted bent 150 degrees geometry to one Zr(1) and one C(6) atom. In the second O site, O(3) is bonded in a single-bond geometry to one Zr(1), two equivalent Zr(2), and one H(1) atom. In the third O site, O(4) is bonded in a bent 150 degrees geometry to one Zr(2) and one H(2) atom. In the fourth O site, O(1) is bonded in a distorted bent 150 degrees geometry to one Zr(2) and one C(6) atom. I(1) is bonded in a 3-coordinate geometry to three equivalent Cu(1) atoms. Linkers: 8 [O]C(=O)c1ccncc1. Metal clusters: 1 O[Zr]1(O)O[C]O[Zr]23(O)(O)O[C]O[Zr](O)(O)O[C]O[Zr](O)(O)(O[C]O1)(O[C]O[Zr](O)(O)(O)O[C]O2)O[C]O[Zr](O)(O)(O)(O)O[C]O3.[OH] ,2 I[Cu@]12[Cu@]3(I)[Cu@@]1(I)[Cu@]23I. The MOF has largest included sphere 13.68 A, density 1.02 g/cm3, surface area 2636.69 m2/g, accessible volume 0.69 cm3/g