AgC5H3SO3 crystallizes in the triclinic P-1 space group. Ag(1) is bonded in a 5-coordinate geometry to one C(4), one C(5), one O(1), one O(2), and one O(3) atom. The Ag(1)-C(4) bond length is 2.35 Å. The Ag(1)-C(5) bond length is 2.41 Å. The Ag(1)-O(1) bond length is 2.34 Å. The Ag(1)-O(2) bond length is 2.44 Å. The Ag(1)-O(3) bond length is 2.43 Å. There are five inequivalent C sites. In the first C site, C(1) is bonded in a distorted single-bond geometry to one C(2) and one H(1) atom. The C(1)-C(2) bond length is 1.38 Å. The C(1)-H(1) bond length is 1.08 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one S(1) atom. The C(2)-C(3) bond length is 1.43 Å. The C(2)-S(1) bond length is 1.79 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(3), and one C(4) atom. The C(3)-C(3) bond length is 1.44 Å. The C(3)-C(4) bond length is 1.43 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one Ag(1), one C(3), and one H(2) atom. The C(4)-H(2) bond length is 1.09 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one Ag(1) and one H(3) atom. The C(5)-H(3) bond length is 1.09 Å. There are three 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(5) atom. S(1) is bonded in a distorted trigonal non-coplanar geometry to one C(2), one O(1), one O(2), and one O(3) atom. The S(1)-O(1) bond length is 1.48 Å. The S(1)-O(2) bond length is 1.47 Å. The S(1)-O(3) bond length is 1.47 Å. There are three inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ag(1) and one S(1) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Ag(1) and one S(1) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Ag(1) and one S(1) atom. Linkers: 2 [O]S([O])([O])c1cccc2c(S([O])([O])[O])c[c]cc12 ,1 [O]S([O])([O])c1cccc2c(S([O])([O])[O])cccc12. Metal clusters: 2 [Ag]. The MOF has largest included sphere 1.37 A, density 2.96 g/cm3, surface area 2189.46 m2/g, accessible volume 0.06 cm3/g