Cu6C65H29(NO6)4 crystallizes in the orthorhombic Cmcm space group. There are three inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a distorted rectangular see-saw-like geometry to one O(3), one O(4), one O(5), and one O(6) atom. The Cu(1)-O(3) bond length is 1.97 Å. The Cu(1)-O(4) bond length is 1.95 Å. The Cu(1)-O(5) bond length is 1.95 Å. The Cu(1)-O(6) bond length is 1.94 Å. In the second Cu site, Cu(2) is bonded in a distorted rectangular see-saw-like geometry to four equivalent O(1) atoms. All Cu(2)-O(1) bond lengths are 1.98 Å. In the third Cu site, Cu(3) is bonded in a rectangular see-saw-like geometry to four equivalent O(2) atoms. All Cu(3)-O(2) bond lengths are 1.93 Å. There are nineteen inequivalent C sites. In the first C site, C(16) is bonded in a distorted single-bond geometry to two equivalent C(12) and one H(8) atom. Both C(16)-C(12) bond lengths are 1.38 Å. The C(16)-H(8) bond length is 0.95 Å. In the second C site, C(17) is bonded in a trigonal planar geometry to one C(18) and two equivalent C(13) atoms. The C(17)-C(18) bond length is 1.49 Å. Both C(17)-C(13) bond lengths are 1.39 Å. In the third C site, C(18) is bonded to one C(17), one C(19), and two equivalent C(14) atoms to form distorted corner-sharing CC4 tetrahedra. The C(18)-C(19) bond length is 1.31 Å. Both C(18)-C(14) bond lengths are 1.50 Å. In the fourth C site, C(1) is bonded in a bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.49 Å. The C(1)-O(1) bond length is 1.25 Å. The C(1)-O(2) bond length is 1.28 Å. In the fifth C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(7) atom. The C(2)-C(3) bond length is 1.39 Å. The C(2)-C(7) bond length is 1.36 Å. In the sixth C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(1) atom. The C(3)-C(4) bond length is 1.40 Å. The C(3)-H(1) bond length is 0.95 Å. In the seventh C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(5), and one C(9) atom. The C(4)-C(5) bond length is 1.39 Å. The C(4)-C(9) bond length is 1.48 Å. In the eighth C site, C(5) is bonded in a distorted single-bond geometry to one C(4), one C(6), and one H(2) atom. The C(5)-C(6) bond length is 1.38 Å. The C(5)-H(2) bond length is 0.95 Å. In the ninth C site, C(6) is bonded in a trigonal planar geometry to one C(5), one C(7), and one C(8) atom. The C(6)-C(7) bond length is 1.40 Å. The C(6)-C(8) bond length is 1.51 Å. In the tenth C site, C(7) is bonded in a distorted single-bond geometry to one C(2), one C(6), and one H(3) atom. The C(7)-H(3) bond length is 0.95 Å. In the eleventh C site, C(8) is bonded in a bent 120 degrees geometry to one C(6), one O(3), and one O(4) atom. The C(8)-O(3) bond length is 1.24 Å. The C(8)-O(4) bond length is 1.24 Å. In the twelfth C site, C(9) is bonded in a trigonal planar geometry to one C(10), one C(15), and one C(4) atom. The C(9)-C(10) bond length is 1.40 Å. The C(9)-C(15) bond length is 1.38 Å. In the thirteenth C site, C(10) is bonded in a distorted trigonal planar geometry to one C(9), one N(1), and one H(4) atom. The C(10)-N(1) bond length is 1.34 Å. The C(10)-H(4) bond length is 0.95 Å. In the fourteenth C site, C(11) is bonded in a bent 120 degrees geometry to one C(12), one O(5), and one O(6) atom. The C(11)-C(12) bond length is 1.50 Å. The C(11)-O(5) bond length is 1.26 Å. The C(11)-O(6) bond length is 1.25 Å. In the fifteenth C site, C(12) is bonded in a trigonal planar geometry to one C(11), one C(13), and one C(16) atom. The C(12)-C(13) bond length is 1.39 Å. In the sixteenth C site, C(13) is bonded in a distorted single-bond geometry to one C(12), one C(17), and one H(5) atom. The C(13)-H(5) bond length is 0.95 Å. In the seventeenth C site, C(14) is bonded in a 2-coordinate geometry to one C(18), one N(2), and one H(6) atom. The C(14)-N(2) bond length is 1.30 Å. The C(14)-H(6) bond length is 0.95 Å. In the eighteenth C site, C(19) is bonded in a distorted trigonal planar geometry to two equivalent C(18) and one H(9) atom. The C(19)-H(9) bond length is 0.95 Å. In the nineteenth C site, C(15) is bonded in a single-bond geometry to two equivalent C(9) and one H(7) atom. The C(15)-H(7) bond length is 0.95 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a bent 120 degrees geometry to two equivalent C(10) atoms. In the second N site, N(2) is bonded in a bent 120 degrees geometry to two equivalent C(14) atoms. There are nine inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(5) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(10) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(13) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(14) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(15) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(16) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(19) atom. There are six inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Cu(2) and one C(1) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Cu(3) and one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(8) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(8) atom. In the fifth O site, O(5) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(11) atom. In the sixth O site, O(6) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(11) atom. Linkers: 4 [O]C(=O)c1cc(C([O])=O)cc([C@]23[CH][C@]4(c5cc(C([O])=O)cc(C([O])=O)c5)[C@@H]5[N][C@H]2[C@H]3[N][C@@H]54)c1 ,11 [O]C(=O)c1cc(C([O])=O)cc(-c2cncc(-c3cc(C([O])=O)cc(C([O])=O)c3)c2)c1. Metal clusters: 12 [C]1O[Cu]234O[C]O[Cu]2(O1)(O[C]O3)O[C]O4. The MOF has largest included sphere 12.34 A, density 0.71 g/cm3, surface area 3785.57 m2/g, accessible volume 1.03 cm3/g