Cd2C6H5S(NO)5 crystallizes in the triclinic P-1 space group. There are three inequivalent Cd sites. In the first Cd site, Cd(1) is bonded to one N(1), one N(2), one N(3), one O(1), one O(2), and one O(3) atom to form CdN3O3 octahedra that share  a cornercorner with one Cd(2)N2O4 octahedra,  a cornercorner with one Cd(3)N2O4 octahedra, and corners with two equivalent S(1)O4 tetrahedra. The corner-sharing octahedral tilt angles are 66°. The Cd(1)-N(1) bond length is 2.36 Å. The Cd(1)-N(2) bond length is 2.43 Å. The Cd(1)-N(3) bond length is 2.53 Å. The Cd(1)-O(1) bond length is 2.28 Å. The Cd(1)-O(2) bond length is 2.26 Å. The Cd(1)-O(3) bond length is 2.36 Å. In the second Cd site, Cd(2) is bonded to two equivalent N(4), two equivalent O(1), and two equivalent O(5) atoms to form CdN2O4 octahedra that share corners with two equivalent Cd(3)N2O4 octahedra, corners with two equivalent Cd(1)N3O3 octahedra, and corners with two equivalent S(1)O4 tetrahedra. The corner-sharing octahedral tilt angles range from 66-78°. Both Cd(2)-N(4) bond lengths are 2.35 Å. Both Cd(2)-O(1) bond lengths are 2.32 Å. Both Cd(2)-O(5) bond lengths are 2.31 Å. In the third Cd site, Cd(3) is bonded to two equivalent N(5), two equivalent O(1), and two equivalent O(4) atoms to form CdN2O4 octahedra that share corners with two equivalent Cd(2)N2O4 octahedra, corners with two equivalent Cd(1)N3O3 octahedra, and corners with two equivalent S(1)O4 tetrahedra. The corner-sharing octahedral tilt angles range from 66-78°. Both Cd(3)-N(5) bond lengths are 2.37 Å. Both Cd(3)-O(1) bond lengths are 2.29 Å. Both Cd(3)-O(4) bond lengths are 2.37 Å. There are six inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(3), one N(1), and one H(1) atom. The C(1)-C(3) bond length is 1.40 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(6), one N(1), and one H(2) atom. The C(2)-C(6) bond length is 1.39 Å. The C(2)-N(1) 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 trigonal planar geometry to one C(1), one C(4), and one C(5) atom. The C(3)-C(4) bond length is 1.47 Å. The C(3)-C(5) bond length is 1.40 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(3), one N(2), and one N(3) atom. The C(4)-N(2) bond length is 1.35 Å. The C(4)-N(3) bond length is 1.35 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(3) and one H(3) atom. The C(5)-H(3) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(2) and one H(4) atom. The C(6)-H(4) bond length is 1.09 Å. There are five inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Cd(1), one C(1), and one C(2) atom. In the second N site, N(2) is bonded in a 3-coordinate geometry to one Cd(1), one C(4), and one N(5) atom. The N(2)-N(5) bond length is 1.34 Å. In the third N site, N(3) is bonded in a distorted single-bond geometry to one Cd(1), one C(4), and one N(4) atom. The N(3)-N(4) bond length is 1.34 Å. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one Cd(2), one N(3), and one N(5) atom. The N(4)-N(5) bond length is 1.31 Å. In the fifth N site, N(5) is bonded in a trigonal planar geometry to one Cd(3), one N(2), and one N(4) atom. There are five 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(5) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(6) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one O(1) atom. The H(5)-O(1) bond length is 0.98 Å. S(1) is bonded to one O(2), one O(3), one O(4), and one O(5) atom to form SO4 tetrahedra that share  a cornercorner with one Cd(2)N2O4 octahedra,  a cornercorner with one Cd(3)N2O4 octahedra, and corners with two equivalent Cd(1)N3O3 octahedra. The corner-sharing octahedral tilt angles range from 34-62°. The S(1)-O(2) bond length is 1.49 Å. The S(1)-O(3) bond length is 1.49 Å. The S(1)-O(4) bond length is 1.49 Å. The S(1)-O(5) bond length is 1.50 Å. There are five inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Cd(1), one Cd(2), one Cd(3), and one H(5) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Cd(1) and one S(1) atom. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one Cd(1) and one S(1) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Cd(3) and one S(1) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Cd(2) and one S(1) atom. Linkers: 2 c1cncc(C2=NN=N[N]2)c1. Metal clusters: 4 [Cd]. The MOF has largest included sphere 1.97 A, density 2.85 g/cm3, surface area 2535.40 m2/g, accessible volume 0.06 cm3/g