AlH5(C2O)5(CH)2 crystallizes in the tetragonal P4/nmm space group. The structure consists of sixteen 02329_fluka molecules inside a AlH5(C2O)5 framework. In the AlH5(C2O)5 framework, there are two inequivalent Al sites. In the first Al site, Al(1) is bonded to two equivalent O(3) and four equivalent O(1) atoms to form corner-sharing AlO6 octahedra. The corner-sharing octahedral tilt angles are 59°. Both Al(1)-O(3) bond lengths are 2.10 Å. All Al(1)-O(1) bond lengths are 1.84 Å. In the second Al site, Al(2) is bonded to two equivalent O(3) and four equivalent O(2) atoms to form corner-sharing AlO6 octahedra. The corner-sharing octahedral tilt angles are 59°. Both Al(2)-O(3) bond lengths are 1.70 Å. All Al(2)-O(2) bond lengths are 1.83 Å. There are five inequivalent C sites. In the first C site, C(1) is bonded in a 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 1.22 Å. The C(1)-O(2) bond length is 1.29 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(4) atom. The C(2)-C(3) bond length is 1.46 Å. The C(2)-C(4) bond length is 1.35 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(3), and one C(5) atom. The C(3)-C(3) bond length is 1.43 Å. The C(3)-C(5) bond length is 1.45 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(2) and one H(1) atom. The C(4)-H(1) bond length is 1.05 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(3) and one H(2) atom. The C(5)-H(2) bond length is 1.10 Å. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(4) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(5) atom. In the third H site, H(4) is bonded in a single-bond geometry to one O(3) atom. The H(4)-O(3) bond length is 0.71 Å. There are three inequivalent O sites. In the first O site, O(1) is bonded in a bent 150 degrees geometry to one Al(1) and one C(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Al(2) and one C(1) atom. In the third O site, O(3) is bonded in a 3-coordinate geometry to one Al(1), one Al(2), and one H(4) atom. Linkers: 8 [O]C(=O)c1ccc(C([O])=O)c2ccccc12. Metal clusters: 8 [Al]. The MOF has largest included sphere 7.82 A, density 1.17 g/cm3, surface area 3755.83 m2/g, accessible volume 0.38 cm3/g