NiCdH4(C3O4)2 crystallizes in the trigonal R-3c space group. Ni(1) is bonded in a rectangular see-saw-like geometry to two equivalent O(2) and two equivalent O(4) atoms. Both Ni(1)-O(2) bond lengths are 2.07 Å. Both Ni(1)-O(4) bond lengths are 2.05 Å. Cd(1) is bonded in a 8-coordinate geometry to two equivalent O(1), two equivalent O(2), two equivalent O(3), and two equivalent O(4) atoms. Both Cd(1)-O(1) bond lengths are 2.25 Å. Both Cd(1)-O(2) bond lengths are 2.68 Å. Both Cd(1)-O(3) bond lengths are 2.30 Å. Both Cd(1)-O(4) bond lengths are 2.57 Å. There are three inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.51 Å. The C(1)-O(1) bond length is 1.27 Å. The C(1)-O(2) bond length is 1.25 Å. In the second C site, C(2) is bonded in a water-like geometry to one C(1) and two equivalent H(1,2) atoms. Both C(2)-H(1,2) bond lengths are 0.97 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one O(3) and one O(4) atom. The C(3)-O(3) bond length is 1.25 Å. The C(3)-O(4) bond length is 1.26 Å. H(1,2) is bonded in a single-bond geometry to one C(2) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a water-like geometry to one Cd(1) and one C(1) atom. In the second O site, O(2) is bonded in a 2-coordinate geometry to one Ni(1), one Cd(1), and one C(1) atom. In the third O site, O(3) is bonded in a water-like geometry to one Cd(1) and one C(3) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Ni(1), one Cd(1), and one C(3) atom. Linkers: 12 [O]C(=O)CC([O])=O. Metal clusters: 6 [Cd] ,6 [Ni]. The MOF has largest included sphere 4.91 A, density 1.86 g/cm3, surface area 2956.47 m2/g, accessible volume 0.21 cm3/g