DyCdH12(C4O5)3 crystallizes in the cubic Fd-3c space group. Dy(1) is bonded in a 9-coordinate geometry to three equivalent O(3) and six equivalent O(1) atoms. All Dy(1)-O(3) bond lengths are 2.44 Å. All Dy(1)-O(1) bond lengths are 2.37 Å. Cd(1) is bonded in an octahedral geometry to six equivalent O(2) atoms. All Cd(1)-O(2) bond lengths are 2.27 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal non-coplanar geometry to one H(1), one H(2), and one O(3) atom. The C(1)-H(1) bond length is 0.97 Å. The C(1)-H(2) bond length is 0.97 Å. The C(1)-O(3) bond length is 1.38 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(2)-O(1) bond length is 1.25 Å. The C(2)-O(2) bond length is 1.26 Å. There are two inequivalent H sites. In the first H site, H(2) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(1) is bonded in a single-bond geometry to one C(1) atom. There are three inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Dy(1) and one C(2) atom. In the second O site, O(2) is bonded in a distorted bent 150 degrees geometry to one Cd(1) and one C(2) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Dy(1) and two equivalent C(1) atoms. Linkers: 96 [O]C(=O)COCC([O])=O. Metal clusters: 32 [Dy] ,32 [Cd]. The MOF has largest included sphere 5.84 A, density 1.97 g/cm3, surface area 2916.11 m2/g, accessible volume 0.20 cm3/g