Cu4C25H24I4(NO)4 crystallizes in the triclinic P-1 space group. The structure consists of a Cu4C25H24I4(NO)4 framework. There are four inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a distorted single-bond geometry to one N(1), one I(1), one I(2), and one I(4) atom. The Cu(1)-N(1) bond length is 2.00 Å. The Cu(1)-I(1) bond length is 2.67 Å. The Cu(1)-I(2) bond length is 2.81 Å. The Cu(1)-I(4) bond length is 2.73 Å. In the second Cu site, Cu(2) is bonded in a distorted single-bond geometry to one N(2), one I(1), one I(2), and one I(3) atom. The Cu(2)-N(2) bond length is 2.00 Å. The Cu(2)-I(1) bond length is 2.81 Å. The Cu(2)-I(2) bond length is 2.65 Å. The Cu(2)-I(3) bond length is 2.73 Å. In the third Cu site, Cu(3) is bonded in a distorted single-bond geometry to one N(3), one I(1), one I(3), and one I(4) atom. The Cu(3)-N(3) bond length is 2.01 Å. The Cu(3)-I(1) bond length is 2.71 Å. The Cu(3)-I(3) bond length is 2.67 Å. The Cu(3)-I(4) bond length is 2.81 Å. In the fourth Cu site, Cu(4) is bonded in a distorted single-bond geometry to one N(4), one I(2), one I(3), and one I(4) atom. The Cu(4)-N(4) bond length is 2.00 Å. The Cu(4)-I(2) bond length is 2.75 Å. The Cu(4)-I(3) bond length is 2.80 Å. The Cu(4)-I(4) bond length is 2.66 Å. There are twenty-five inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(13), one N(1), and one H(1) atom. The C(1)-C(13) bond length is 1.39 Å. The C(1)-N(1) bond length is 1.35 Å. The C(1)-H(1) bond length is 1.09 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(14), one N(2), and one H(2) atom. The C(2)-C(14) bond length is 1.39 Å. The C(2)-N(2) bond length is 1.35 Å. The C(2)-H(2) bond length is 1.09 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(15), one N(3), and one H(3) atom. The C(3)-C(15) bond length is 1.39 Å. The C(3)-N(3) bond length is 1.35 Å. The C(3)-H(3) bond length is 1.09 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(16), one N(4), and one H(4) atom. The C(4)-C(16) bond length is 1.39 Å. The C(4)-N(4) bond length is 1.35 Å. The C(4)-H(4) bond length is 1.09 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(5,6) atom. The C(5)-N(1) bond length is 1.34 Å. The C(5)-H(5,6) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(5,6) atom. The C(6)-N(2) bond length is 1.34 Å. The C(6)-H(5,6) bond length is 1.09 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(7) atom. The C(7)-N(3) bond length is 1.34 Å. The C(7)-H(7) bond length is 1.09 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one N(4) and one H(8) atom. The C(8)-N(4) bond length is 1.34 Å. The C(8)-H(8) bond length is 1.09 Å. In the ninth C site, C(9) is bonded in a distorted single-bond geometry to one C(22) and one O(1) atom. The C(9)-C(22) bond length is 1.40 Å. The C(9)-O(1) bond length is 1.36 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(23) and one O(2) atom. The C(10)-C(23) bond length is 1.40 Å. The C(10)-O(2) bond length is 1.36 Å. In the eleventh C site, C(11) is bonded in a distorted single-bond geometry to one C(24) and one O(3) atom. The C(11)-C(24) bond length is 1.40 Å. The C(11)-O(3) bond length is 1.36 Å. In the twelfth C site, C(12) is bonded in a distorted single-bond geometry to one C(25) and one O(4) atom. The C(12)-C(25) bond length is 1.40 Å. The C(12)-O(4) bond length is 1.36 Å. In the thirteenth C site, C(13) is bonded in a distorted single-bond geometry to one C(1); one C(22); and one H(9,10) atom. The C(13)-C(22) bond length is 1.39 Å. The C(13)-H(9,10) bond length is 1.09 Å. In the fourteenth C site, C(14) is bonded in a distorted trigonal planar geometry to one C(2); one C(23); and one H(9,10) atom. The C(14)-C(23) bond length is 1.40 Å. The C(14)-H(9,10) bond length is 1.09 Å. In the fifteenth C site, C(15) is bonded in a distorted trigonal planar geometry to one C(24), one C(3), and one H(11) atom. The C(15)-C(24) bond length is 1.40 Å. The C(15)-H(11) bond length is 1.09 Å. In the sixteenth C site, C(16) is bonded in a distorted single-bond geometry to one C(25), one C(4), and one H(12) atom. The C(16)-C(25) bond length is 1.39 Å. The C(16)-H(12) bond length is 1.09 Å. In the seventeenth C site, C(17) is bonded in a tetrahedral geometry to one C(18), one C(19), one C(20), and one C(21) atom. The C(17)-C(18) bond length is 1.53 Å. The C(17)-C(19) bond length is 1.53 Å. The C(17)-C(20) bond length is 1.53 Å. The C(17)-C(21) bond length is 1.53 Å. In the eighteenth C site, C(18) is bonded in a distorted trigonal non-coplanar geometry to one C(17), one H(13), one H(17), and one O(1) atom. The C(18)-H(13) bond length is 1.10 Å. The C(18)-H(17) bond length is 1.10 Å. The C(18)-O(1) bond length is 1.44 Å. In the nineteenth C site, C(19) is bonded in a distorted trigonal non-coplanar geometry to one C(17), one H(14), one H(18), and one O(2) atom. The C(19)-H(14) bond length is 1.10 Å. The C(19)-H(18) bond length is 1.10 Å. The C(19)-O(2) bond length is 1.44 Å. In the twentieth C site, C(20) is bonded in a distorted trigonal non-coplanar geometry to one C(17), one H(15), one H(19), and one O(3) atom. The C(20)-H(15) bond length is 1.10 Å. The C(20)-H(19) bond length is 1.10 Å. The C(20)-O(3) bond length is 1.44 Å. In the twenty-first C site, C(21) is bonded in a distorted trigonal non-coplanar geometry to one C(17), one H(16), one H(20), and one O(4) atom. The C(21)-H(16) bond length is 1.10 Å. The C(21)-H(20) bond length is 1.10 Å. The C(21)-O(4) bond length is 1.44 Å. In the twenty-second C site, C(22) is bonded in a distorted trigonal planar geometry to one C(13), one C(9), and one H(21) atom. The C(22)-H(21) bond length is 1.09 Å. In the twenty-third C site, C(23) is bonded in a distorted trigonal planar geometry to one C(10), one C(14), and one H(22) atom. The C(23)-H(22) bond length is 1.09 Å. In the twenty-fourth C site, C(24) is bonded in a distorted trigonal planar geometry to one C(11), one C(15), and one H(23) atom. The C(24)-H(23) bond length is 1.09 Å. In the twenty-fifth C site, C(25) is bonded in a distorted trigonal planar geometry to one C(12), one C(16), and one H(24) atom. The C(25)-H(24) bond length is 1.09 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(5) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Cu(2), one C(2), and one C(6) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Cu(3), one C(3), and one C(7) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one Cu(4), one C(4), and one C(8) atom. There are twenty-two 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(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(3) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(4) atom. In the fifth H site, H(5,6) is bonded in a single-bond geometry to one C(5) atom. In the sixth H site, H(7) is bonded in a single-bond geometry to one C(7) atom. In the seventh H site, H(8) is bonded in a single-bond geometry to one C(8) atom. In the eighth H site, H(9,10) is bonded in a single-bond geometry to one C(13) atom. In the ninth H site, H(11) is bonded in a single-bond geometry to one C(15) atom. In the tenth H site, H(12) is bonded in a single-bond geometry to one C(16) atom. In the eleventh H site, H(13) is bonded in a single-bond geometry to one C(18) atom. In the twelfth H site, H(14) is bonded in a single-bond geometry to one C(19) atom. In the thirteenth H site, H(15) is bonded in a single-bond geometry to one C(20) atom. In the fourteenth H site, H(16) is bonded in a single-bond geometry to one C(21) atom. In the fifteenth H site, H(17) is bonded in a single-bond geometry to one C(18) atom. In the sixteenth H site, H(18) is bonded in a single-bond geometry to one C(19) atom. In the seventeenth H site, H(19) is bonded in a single-bond geometry to one C(20) atom. In the eighteenth H site, H(20) is bonded in a single-bond geometry to one C(21) atom. In the nineteenth H site, H(21) is bonded in a single-bond geometry to one C(22) atom. In the twentieth H site, H(22) is bonded in a single-bond geometry to one C(23) atom. In the twenty-first H site, H(23) is bonded in a single-bond geometry to one C(24) atom. In the twenty-second H site, H(24) is bonded in a single-bond geometry to one C(25) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one C(18) and one C(9) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one C(10) and one C(19) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one C(11) and one C(20) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one C(12) and one C(21) atom. There are four inequivalent I sites. In the first I site, I(1) is bonded in a 3-coordinate geometry to one Cu(1), one Cu(2), and one Cu(3) atom. In the second I site, I(2) is bonded in a 3-coordinate geometry to one Cu(1), one Cu(2), and one Cu(4) atom. In the third I site, I(3) is bonded in a 3-coordinate geometry to one Cu(2), one Cu(3), and one Cu(4) atom. In the fourth I site, I(4) is bonded in a 3-coordinate geometry to one Cu(1), one Cu(3), and one Cu(4) atom. Linkers: 2 c1cncc(OCC(COc2cccnc2)(COc2cccnc2)COc2cccnc2)c1. Metal clusters: 2 I[Cu@]12[Cu@]3(I)[Cu@@]1(I)[Cu@]23I. The MOF has largest included sphere 2.47 A, density 2.57 g/cm3, surface area 2781.54 m2/g, accessible volume 0.12 cm3/g