Gd(CO2)3CH2 crystallizes in the triclinic P-1 space group. The structure consists of two 02329_fluka molecules inside a Gd(CO2)3 framework. In the Gd(CO2)3 framework, Gd(1) is bonded in a 9-coordinate geometry to one O(1), one O(2), one O(5), two equivalent O(3), two equivalent O(4), and two equivalent O(6) atoms. The Gd(1)-O(1) bond length is 2.37 Å. The Gd(1)-O(2) bond length is 2.42 Å. The Gd(1)-O(5) bond length is 2.33 Å. There is one shorter (2.47 Å) and one longer (2.51 Å) Gd(1)-O(3) bond length. There is one shorter (2.42 Å) and one longer (2.64 Å) Gd(1)-O(4) bond length. There is one shorter (2.45 Å) and one longer (2.46 Å) Gd(1)-O(6) bond length. There are three inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one O(2) and one O(3) atom. The C(1)-O(2) bond length is 1.26 Å. The C(1)-O(3) bond length is 1.30 Å. In the second C site, C(3) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(5) atom. The C(3)-O(1) bond length is 1.26 Å. The C(3)-O(5) bond length is 1.27 Å. In the third C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(4) and one O(6) atom. The C(4)-O(4) bond length is 1.27 Å. The C(4)-O(6) bond length is 1.29 Å. There are six inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Gd(1) and one C(3) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Gd(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to two equivalent Gd(1) and one C(1) atom. In the fourth O site, O(4) is bonded in a distorted single-bond geometry to two equivalent Gd(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Gd(1) and one C(3) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to two equivalent Gd(1) and one C(4) atom. Linkers: 1 [O]C(=O)C([O])=O ,2 [O]C(=O)CC([O])=O. Metal clusters: 2 [Gd]. RCSR code: tcs. The MOF has largest included sphere 1.93 A, density 3.46 g/cm3, surface area 1600.22 m2/g, accessible volume 0.05 cm3/g