Cu2C4H6S(NO)8 crystallizes in the orthorhombic Fdd2 space group. Cu(1) is bonded to one N(2), one N(4), one O(1), one O(2), and one O(3) atom to form CuN2O3 square pyramids that share  a cornercorner with one S(1)O4 tetrahedra. The Cu(1)-N(2) bond length is 1.94 Å. The Cu(1)-N(4) bond length is 2.14 Å. The Cu(1)-O(1) bond length is 1.94 Å. The Cu(1)-O(2) bond length is 2.35 Å. The Cu(1)-O(3) bond length is 2.01 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one N(2), one N(3), and one O(1) atom. The C(1)-N(2) bond length is 1.33 Å. The C(1)-N(3) bond length is 1.38 Å. The C(1)-O(1) bond length is 1.27 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one N(1), one N(3), and one O(2) atom. The C(2)-N(1) bond length is 1.38 Å. The C(2)-N(3) bond length is 1.40 Å. The C(2)-O(2) bond length is 1.23 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a 2-coordinate geometry to one C(2), one N(2), and one H(1) atom. The N(1)-N(2) bond length is 1.41 Å. The N(1)-H(1) bond length is 1.02 Å. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one Cu(1), one C(1), and one N(1) atom. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one C(1), one C(2), and one N(4) atom. The N(3)-N(4) bond length is 1.40 Å. In the fourth N site, N(4) is bonded in a distorted water-like geometry to one Cu(1), one N(3), one H(2), and one H(3) atom. The N(4)-H(2) bond length is 1.05 Å. The N(4)-H(3) bond length is 1.04 Å. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one N(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one N(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one N(4) atom. S(1) is bonded to two equivalent O(3) and two equivalent O(4) atoms to form SO4 tetrahedra that share corners with two equivalent Cu(1)N2O3 square pyramids. Both S(1)-O(3) bond lengths are 1.54 Å. Both S(1)-O(4) bond lengths are 1.47 Å. There are four inequivalent O sites. In the first O site, O(1) is bonded in a water-like geometry to one Cu(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(2) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Cu(1) and one S(1) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one S(1) atom. Linkers: 4 NN1C(=O)[N]NC1=O ,2 [O]S([O])(=O)=O. Metal clusters: 4 [Cu]. The MOF has largest included sphere 2.08 A, density 2.46 g/cm3, surface area 2760.03 m2/g, accessible volume 0.08 cm3/g