Cu3C10H6I2(NO)4 crystallizes in the orthorhombic Pbcn space group. There are three inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a distorted single-bond geometry to one N(4), one I(1), and two equivalent I(2) atoms. The Cu(1)-N(4) bond length is 2.09 Å. The Cu(1)-I(1) bond length is 2.65 Å. There is one shorter (2.65 Å) and one longer (2.66 Å) Cu(1)-I(2) bond length. In the second Cu site, Cu(2) is bonded in a 4-coordinate geometry to one N(3), one I(2), and two equivalent I(1) atoms. The Cu(2)-N(3) bond length is 2.10 Å. The Cu(2)-I(2) bond length is 2.71 Å. There is one shorter (2.63 Å) and one longer (2.65 Å) Cu(2)-I(1) bond length. In the third Cu site, Cu(3) is bonded in a square co-planar geometry to one N(1), one N(2), one O(1), and one O(2) atom. The Cu(3)-N(1) bond length is 2.00 Å. The Cu(3)-N(2) bond length is 2.01 Å. The Cu(3)-O(1) bond length is 1.93 Å. The Cu(3)-O(2) bond length is 1.96 Å. There are ten inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(4), one N(1), and one H(1) atom. The C(1)-C(4) bond length is 1.38 Å. The C(1)-N(1) bond length is 1.33 Å. The C(1)-H(1) bond length is 0.93 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(2), and one O(4) atom. The C(2)-C(5) bond length is 1.49 Å. The C(2)-O(2) bond length is 1.29 Å. The C(2)-O(4) bond length is 1.23 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(3) atom. The C(3)-O(1) bond length is 1.27 Å. The C(3)-O(3) bond length is 1.23 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(1), one N(3), and one H(2) atom. The C(4)-N(3) bond length is 1.35 Å. The C(4)-H(2) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(2), one C(6), and one N(2) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-N(2) bond length is 1.35 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(5), one N(4), and one H(3) atom. The C(6)-N(4) bond length is 1.34 Å. The C(6)-H(3) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(8), one N(4), and one H(4) atom. The C(7)-C(8) bond length is 1.35 Å. The C(7)-N(4) bond length is 1.34 Å. The C(7)-H(4) bond length is 0.93 Å. In the eighth C site, C(8) is bonded in a distorted trigonal planar geometry to one C(7), one N(2), and one H(5) atom. The C(8)-N(2) bond length is 1.33 Å. The C(8)-H(5) bond length is 0.93 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(6) atom. The C(9)-N(3) bond length is 1.34 Å. The C(9)-H(6) bond length is 0.93 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one N(1) atom. The C(10)-N(1) bond length is 1.33 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Cu(3), one C(1), and one C(10) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Cu(3), one C(5), and one C(8) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Cu(2), one C(4), and one C(9) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one Cu(1), one C(6), and one C(7) atom. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(6) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(7) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(8) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(9) atom. There are four inequivalent O sites. In the first O site, O(2) is bonded in a bent 120 degrees geometry to one Cu(3) and one C(2) atom. In the second O site, O(3) is bonded in a single-bond geometry to one C(3) atom. In the third O site, O(4) is bonded in a single-bond geometry to one C(2) atom. In the fourth O site, O(1) is bonded in a bent 120 degrees geometry to one Cu(3) and one C(3) atom. There are two inequivalent I sites. In the first I site, I(1) is bonded in a distorted trigonal non-coplanar geometry to one Cu(1) and two equivalent Cu(2) atoms. In the second I site, I(2) is bonded in a distorted trigonal planar geometry to one Cu(2) and two equivalent Cu(1) atoms. Linkers: 16 [O]C(=O)c1cnccn1. Metal clusters: 24 [Cu]. The MOF has largest included sphere 4.67 A, density 2.42 g/cm3, surface area 2602.57 m2/g, accessible volume 0.16 cm3/g