Gd2CuC10N4H4O9 crystallizes in the trigonal R-3 space group. Gd(1) is bonded in a 9-coordinate geometry to one N(2), one O(2), one O(5), one O(6), two equivalent O(1), and three equivalent O(4) atoms. The Gd(1)-N(2) bond length is 2.56 Å. The Gd(1)-O(2) bond length is 2.44 Å. The Gd(1)-O(5) bond length is 2.60 Å. The Gd(1)-O(6) bond length is 2.25 Å. There is one shorter (2.41 Å) and one longer (2.61 Å) Gd(1)-O(1) bond length. There are a spread of Gd(1)-O(4) bond distances ranging from 2.34-2.44 Å. Cu(1) is bonded in a square co-planar geometry to two equivalent N(1) and two equivalent O(3) atoms. Both Cu(1)-N(1) bond lengths are 1.97 Å. Both Cu(1)-O(3) bond lengths are 1.94 Å. There are five inequivalent C sites. In the first C site, C(2) is bonded in a distorted trigonal planar geometry to one C(4), one N(1), and one H(1) atom. The C(2)-C(4) bond length is 1.38 Å. The C(2)-N(1) bond length is 1.34 Å. The C(2)-H(1) bond length is 0.93 Å. In the second C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(2), and one O(3) atom. The C(3)-C(1) bond length is 1.50 Å. The C(3)-O(2) bond length is 1.24 Å. The C(3)-O(3) bond length is 1.26 Å. In the third C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(2), one N(2), and one H(2) atom. The C(4)-N(2) bond length is 1.31 Å. The C(4)-H(2) bond length is 0.93 Å. In the fourth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(1), one N(2), and one O(1) atom. The C(5)-C(1) bond length is 1.42 Å. The C(5)-N(2) bond length is 1.36 Å. The C(5)-O(1) bond length is 1.27 Å. In the fifth C site, C(1) is bonded in a distorted trigonal planar geometry to one C(3), one C(5), and one N(1) atom. The C(1)-N(1) bond length is 1.34 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(2) atom. In the second N site, N(2) is bonded in a 3-coordinate geometry to one Gd(1), one C(4), and one C(5) atom. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(4) atom. There are six inequivalent O sites. In the first O site, O(3) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(3) atom. In the second O site, O(4) is bonded in a trigonal non-coplanar geometry to three equivalent Gd(1) atoms. In the third O site, O(5) is bonded in an octahedral geometry to six equivalent Gd(1) atoms. In the fourth O site, O(6) is bonded in a trigonal non-coplanar geometry to three equivalent Gd(1) atoms. In the fifth O site, O(1) is bonded in a 3-coordinate geometry to two equivalent Gd(1) and one C(5) atom. In the sixth O site, O(2) is bonded in a distorted bent 150 degrees geometry to one Gd(1) and one C(3) atom. Linkers: 6 [O]C(=O)[C]1N=CC=NC1=O. Metal clusters: 6 [Gd] ,3 [Cu]. The MOF has largest included sphere 5.36 A, density 2.29 g/cm3, surface area 1990.40 m2/g, accessible volume 0.23 cm3/g