Gd2Cu3(C4O5)6 crystallizes in the hexagonal P6/mcc space group. Gd(1) is bonded in a 9-coordinate geometry to three equivalent O(3) and six equivalent O(1) atoms. All Gd(1)-O(3) bond lengths are 2.52 Å. All Gd(1)-O(1) bond lengths are 2.45 Å. Cu(1) is bonded in a square co-planar geometry to four equivalent O(2) atoms. All Cu(1)-O(2) bond lengths are 1.96 Å. There are two inequivalent C sites. In the first C site, C(1) is bonded in a single-bond geometry to one O(3) atom. The C(1)-O(3) bond length is 1.41 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 1.23 Å. The C(2)-O(2) bond length is 1.25 Å. There are three inequivalent O sites. In the first O site, O(3) is bonded in a distorted trigonal planar geometry to one Gd(1) and two equivalent C(1) atoms. In the second O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Gd(1) and one C(2) atom. In the third O site, O(2) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(2) atom. Linkers: 12 [O]C(=O)[C]O[C]C([O])=O. Metal clusters: 4 [Gd] ,6 [Cu]. The MOF has largest included sphere 9.09 A, density 1.45 g/cm3, surface area 3102.14 m2/g, accessible volume 0.39 cm3/g