LiH5(C2O)3 crystallizes in the monoclinic C2/c space group. Li(1) is bonded to one O(1), one O(2), and two equivalent O(3) atoms to form distorted edge-sharing LiO4 tetrahedra. The Li(1)-O(1) bond length is 1.95 Å. The Li(1)-O(2) bond length is 1.89 Å. There is one shorter (1.96 Å) and one longer (2.04 Å) Li(1)-O(3) bond length. There are six inequivalent C sites. In the first C site, C(5) is bonded in a distorted trigonal planar geometry to one C(4), one C(6), and one H(4) atom. The C(5)-C(4) bond length is 1.42 Å. The C(5)-C(6) bond length is 1.38 Å. The C(5)-H(4) bond length is 1.09 Å. In the second C site, C(6) is bonded in a distorted single-bond geometry to one C(2), one C(5), and one H(5) atom. The C(6)-C(2) bond length is 1.42 Å. The C(6)-H(5) bond length is 1.09 Å. In the third C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(3) atom. The C(1)-C(2) bond length is 1.50 Å. The C(1)-O(1) bond length is 1.27 Å. The C(1)-O(3) bond length is 1.29 Å. In the fourth C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(6) atom. The C(2)-C(3) bond length is 1.39 Å. In the fifth C site, C(3) is bonded in a distorted trigonal planar geometry to one C(2), one C(4), and one H(3) atom. The C(3)-C(4) bond length is 1.41 Å. The C(3)-H(3) bond length is 1.09 Å. In the sixth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(4), and one C(5) atom. The C(4)-C(4) bond length is 1.44 Å. There are five inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(2) atom. The H(1)-O(2) bond length is 0.99 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(2) atom. The H(2)-O(2) bond length is 0.99 Å. In the third H site, H(3) is bonded in a single-bond geometry to one C(3) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(5) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(6) atom. There are three inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Li(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted trigonal non-coplanar geometry to one Li(1), one H(1), and one H(2) atom. In the third O site, O(3) is bonded in a 3-coordinate geometry to two equivalent Li(1) and one C(1) atom. Linkers: 2 [O]C(=O)c1ccc2cc(C([O])=O)ccc2c1. Metal clusters: 4 [Li]. The MOF has largest included sphere 2.09 A, density 1.49 g/cm3, surface area 4489.25 m2/g, accessible volume 0.13 cm3/g