Gd2Co3C42H30(NO5)6 crystallizes in the hexagonal P6/mcc space group. Gd(1) is bonded in a 9-coordinate geometry to three equivalent N(1) and six equivalent O(1) atoms. All Gd(1)-N(1) bond lengths are 2.51 Å. All Gd(1)-O(1) bond lengths are 2.44 Å. Co(1) is bonded in an octahedral geometry to two equivalent O(3) and four equivalent O(2) atoms. Both Co(1)-O(3) bond lengths are 2.12 Å. All Co(1)-O(2) bond lengths are 2.06 Å. There are four inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.50 Å. The C(1)-O(1) bond length is 1.28 Å. The C(1)-O(2) bond length is 1.26 Å. In the second C site, C(4) is bonded in a distorted single-bond geometry to two equivalent C(3) and one H(3) atom. Both C(4)-C(3) bond lengths are 1.39 Å. The C(4)-H(3) bond length is 1.09 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(2), one C(4), and one H(2) atom. The C(3)-C(2) bond length is 1.40 Å. The C(3)-H(2) bond length is 1.09 Å. In the fourth C site, C(2) is bonded in a distorted single-bond geometry to one C(1), one C(3), and one N(1) atom. The C(2)-N(1) bond length is 1.34 Å. N(1) is bonded in a distorted trigonal planar geometry to one Gd(1) and two equivalent C(2) atoms. There are three inequivalent H sites. In the first H site, H(2) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(1) is bonded in a single-bond geometry to one O(3) atom. The H(1)-O(3) bond length is 1.00 Å. In the third H site, H(3) is bonded in a single-bond geometry to one C(4) atom. There are three inequivalent O sites. In the first O site, O(1) is bonded in a distorted single-bond geometry to one Gd(1) and one C(1) atom. In the second O site, O(3) is bonded in a distorted trigonal non-coplanar geometry to one Co(1) and two equivalent H(1) atoms. In the third O site, O(2) is bonded in a bent 120 degrees geometry to one Co(1) and one C(1) atom. Linkers: 12 [O]C(=O)c1cccc(C([O])=O)n1. Metal clusters: 4 [Gd] ,6 [Co]. The MOF has largest included sphere 6.94 A, density 1.70 g/cm3, surface area 3110.63 m2/g, accessible volume 0.22 cm3/g