Ce2Cu3H24(C4O5)6 crystallizes in the hexagonal P-62c space group. Ce(1) is bonded in a 9-coordinate geometry to three equivalent O(1), three equivalent O(2), and three equivalent O(4) atoms. All Ce(1)-O(1) bond lengths are 2.61 Å. All Ce(1)-O(2) bond lengths are 2.54 Å. All Ce(1)-O(4) bond lengths are 2.52 Å. Cu(1) is bonded in a square co-planar geometry to two equivalent O(3) and two equivalent O(5) atoms. Both Cu(1)-O(3) bond lengths are 1.94 Å. Both Cu(1)-O(5) bond lengths are 1.95 Å. There are four 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(1) 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(1) bond length is 1.37 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one O(2) and one O(3) atom. The C(2)-O(2) bond length is 1.25 Å. The C(2)-O(3) bond length is 1.24 Å. In the third C site, C(3) is bonded in a distorted trigonal non-coplanar geometry to two equivalent H(3,4) and one O(1) atom. Both C(3)-H(3,4) bond lengths are 0.97 Å. The C(3)-O(1) bond length is 1.41 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(4) and one O(5) atom. The C(4)-O(4) bond length is 1.24 Å. The C(4)-O(5) bond length is 1.25 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(1) atom. In the third H site, H(3,4) is bonded in a single-bond geometry to one C(3) atom. There are five inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ce(1), one C(1), and one C(3) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Ce(1) and one C(2) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(2) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one Ce(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(4) atom. Linkers: 12 [O]C(=O)COCC([O])=O. Metal clusters: 4 [Ce] ,6 [Cu]. The MOF has largest included sphere 8.46 A, density 1.46 g/cm3, surface area 3318.97 m2/g, accessible volume 0.38 cm3/g