Cd5C20H4(NO2)8 crystallizes in the orthorhombic Pnma space group. There are three inequivalent Cd sites. In the first Cd site, Cd(1) is bonded in a 6-coordinate geometry to one N(2), one N(3), one O(1), one O(4), and two equivalent O(6) atoms. The Cd(1)-N(2) bond length is 2.24 Å. The Cd(1)-N(3) bond length is 2.25 Å. The Cd(1)-O(1) bond length is 2.29 Å. The Cd(1)-O(4) bond length is 2.58 Å. There is one shorter (2.25 Å) and one longer (2.46 Å) Cd(1)-O(6) bond length. In the second Cd site, Cd(2) is bonded to one N(1), one N(4), one O(1), one O(4), and two equivalent O(7) atoms to form distorted edge-sharing CdN2O4 pentagonal pyramids. The Cd(2)-N(1) bond length is 2.27 Å. The Cd(2)-N(4) bond length is 2.26 Å. The Cd(2)-O(1) bond length is 2.47 Å. The Cd(2)-O(4) bond length is 2.34 Å. There is one shorter (2.24 Å) and one longer (2.44 Å) Cd(2)-O(7) bond length. In the third Cd site, Cd(3) is bonded in a rectangular see-saw-like geometry to two equivalent O(5) and two equivalent O(8) atoms. Both Cd(3)-O(5) bond lengths are 2.18 Å. Both Cd(3)-O(8) bond lengths are 2.20 Å. There are eleven inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one N(1), one N(2), and one H(1) atom. The C(1)-N(1) bond length is 1.35 Å. The C(1)-N(2) bond length is 1.33 Å. The C(1)-H(1) bond length is 0.93 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one N(2) atom. The C(2)-N(2) bond length is 1.37 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one N(1) atom. The C(3)-N(1) bond length is 1.37 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(3) and one O(4) atom. The C(4)-O(3) bond length is 1.29 Å. The C(4)-O(4) bond length is 1.23 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(5)-O(1) bond length is 1.23 Å. The C(5)-O(2) bond length is 1.27 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one N(4) atom. The C(6)-N(4) bond length is 1.37 Å. In the seventh C site, C(7) is bonded in a bent 120 degrees geometry to one O(7) and one O(8) atom. The C(7)-O(7) bond length is 1.26 Å. The C(7)-O(8) bond length is 1.23 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one N(3) atom. The C(8)-N(3) bond length is 1.36 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one O(5) and one O(6) atom. The C(9)-O(5) bond length is 1.23 Å. The C(9)-O(6) bond length is 1.26 Å. In the tenth C site, C(10) is bonded in a trigonal planar geometry to two equivalent N(4) and one H(2) atom. Both C(10)-N(4) bond lengths are 1.34 Å. The C(10)-H(2) bond length is 0.93 Å. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to two equivalent N(3) and one H(3) atom. Both C(11)-N(3) bond lengths are 1.32 Å. The C(11)-H(3) bond length is 0.93 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one Cd(2), one C(1), and one C(3) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Cd(1), one C(1), and one C(2) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Cd(1), one C(11), and one C(8) atom. In the fourth N site, N(4) is bonded in a distorted trigonal planar geometry to one Cd(2), one C(10), and one C(6) atom. 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(10) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(11) atom. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a distorted trigonal planar geometry to one Cd(1), one Cd(2), and one C(5) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(5) atom. In the third O site, O(3) is bonded in a single-bond geometry to one C(4) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Cd(1), one Cd(2), and one C(4) atom. In the fifth O site, O(5) is bonded in a distorted bent 150 degrees geometry to one Cd(3) and one C(9) atom. In the sixth O site, O(6) is bonded in a distorted trigonal planar geometry to two equivalent Cd(1) and one C(9) atom. In the seventh O site, O(7) is bonded in a distorted trigonal planar geometry to two equivalent Cd(2) and one C(7) atom. In the eighth O site, O(8) is bonded in a distorted bent 120 degrees geometry to one Cd(3) and one C(7) atom. Linkers: 11 [O]C(=O)C1=C(C([O])=O)N=C[N]1 ,5 [O]C(=O)[C]1N=CN=C1C([O])=O. Metal clusters: 20 [Cd]. The MOF has largest included sphere 5.04 A, density 2.17 g/cm3, surface area 2510.83 m2/g, accessible volume 0.24 cm3/g