Cu3C26H22S2(NO9)2 crystallizes in the monoclinic P2_1/c space group. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a square pyramidal geometry to one O(1), one O(2), one O(3), one O(5), and one O(9) atom. The Cu(1)-O(1) bond length is 2.01 Å. The Cu(1)-O(2) bond length is 2.01 Å. The Cu(1)-O(3) bond length is 1.96 Å. The Cu(1)-O(5) bond length is 2.02 Å. The Cu(1)-O(9) bond length is 2.35 Å. In the second Cu site, Cu(2) is bonded in an octahedral geometry to two equivalent N(1), two equivalent O(6), and two equivalent O(7) atoms. Both Cu(2)-N(1) bond lengths are 1.97 Å. Both Cu(2)-O(6) bond lengths are 2.04 Å. Both Cu(2)-O(7) bond lengths are 2.38 Å. There are thirteen inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(3), and one O(4) atom. The C(1)-C(2) bond length is 1.51 Å. The C(1)-O(3) bond length is 1.29 Å. The C(1)-O(4) bond length is 1.26 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 1.40 Å. The C(2)-C(4) bond length is 1.40 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2) and one H(5) atom. The C(3)-H(5) bond length is 1.09 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(2), one C(6), and one H(6) atom. The C(4)-C(6) bond length is 1.40 Å. The C(4)-H(6) bond length is 1.09 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(7) and one H(7) atom. The C(5)-C(7) bond length is 1.40 Å. The C(5)-H(7) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(4), one C(7), and one S(1) atom. The C(6)-C(7) bond length is 1.41 Å. The C(6)-S(1) bond length is 1.79 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(5), one C(6), and one C(8) atom. The C(7)-C(8) bond length is 1.50 Å. In the eighth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(5), and one O(6) atom. The C(8)-O(5) bond length is 1.29 Å. The C(8)-O(6) bond length is 1.26 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(8) atom. The C(9)-N(1) bond length is 1.34 Å. The C(9)-H(8) bond length is 1.09 Å. In the tenth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one C(11), one N(1), and one H(9) atom. The C(10)-C(11) bond length is 1.39 Å. The C(10)-N(1) bond length is 1.35 Å. The C(10)-H(9) bond length is 1.09 Å. In the eleventh C site, C(11) is bonded in a distorted trigonal planar geometry to one C(10), one C(13), and one H(10) atom. The C(11)-C(13) bond length is 1.41 Å. The C(11)-H(10) bond length is 1.09 Å. In the twelfth C site, C(12) is bonded in a distorted single-bond geometry to one C(13) and one H(11) atom. The C(12)-C(13) bond length is 1.40 Å. The C(12)-H(11) bond length is 1.09 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(11), one C(12), and one C(13) atom. The C(13)-C(13) bond length is 1.48 Å. N(1) is bonded in a trigonal planar geometry to one Cu(2), one C(10), and one C(9) atom. There are eleven inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(1) atom. The H(1)-O(1) bond length is 0.99 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(1) atom. The H(2)-O(1) bond length is 0.99 Å. In the third H site, H(3) is bonded in a single-bond geometry to one O(2) atom. The H(3)-O(2) bond length is 0.99 Å. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(2) and one O(5) atom. The H(4)-O(2) bond length is 1.00 Å. The H(4)-O(5) bond length is 1.74 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(3) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(4) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(5) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(9) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(10) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(11) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(12) atom. S(1) is bonded in a distorted trigonal non-coplanar geometry to one C(6), one O(7), one O(8), and one O(9) atom. The S(1)-O(7) bond length is 1.47 Å. The S(1)-O(8) bond length is 1.49 Å. The S(1)-O(9) bond length is 1.47 Å. There are nine inequivalent O sites. In the first O site, O(6) is bonded in a distorted bent 120 degrees geometry to one Cu(2) and one C(8) atom. In the second O site, O(7) is bonded in a distorted bent 120 degrees geometry to one Cu(2) and one S(1) atom. In the third O site, O(8) is bonded in a single-bond geometry to one S(1) atom. In the fourth O site, O(9) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one S(1) atom. In the fifth O site, O(1) is bonded in a distorted trigonal non-coplanar geometry to one Cu(1), one H(1), and one H(2) atom. In the sixth O site, O(2) is bonded in a distorted trigonal non-coplanar geometry to one Cu(1), one H(3), and one H(4) atom. In the seventh O site, O(3) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(1) atom. In the eighth O site, O(4) is bonded in a single-bond geometry to one C(1) atom. In the ninth O site, O(5) is bonded in a 3-coordinate geometry to one Cu(1), one C(8), and one H(4) atom. Linkers: 4 [O]C(=O)c1ccc(C([O])=O)c(S([O])([O])[O])c1. Metal clusters: 6 [Cu]. The MOF has largest included sphere 2.03 A, density 2.03 g/cm3, surface area 3366.47 m2/g, accessible volume 0.11 cm3/g