DyH3(C3O2)3 crystallizes in the tetragonal P4_122 space group. Dy(1) is bonded in a pentagonal pyramidal geometry to two equivalent O(1), two equivalent O(2), and two equivalent O(3) atoms. Both Dy(1)-O(1) bond lengths are 2.31 Å. Both Dy(1)-O(2) bond lengths are 2.31 Å. Both Dy(1)-O(3) bond lengths are 2.31 Å. There are six inequivalent C sites. In the first C site, C(4) is bonded in a trigonal planar geometry to one C(5) and two equivalent C(1) atoms. The C(4)-C(5) bond length is 1.52 Å. Both C(4)-C(1) bond lengths are 1.39 Å. In the second C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(4) and two equivalent O(2) atoms. Both C(5)-O(2) bond lengths are 1.25 Å. In the third C site, C(6) is bonded in a single-bond geometry to two equivalent C(2) and one H(2) atom. Both C(6)-C(2) bond lengths are 1.39 Å. The C(6)-H(2) bond length is 0.93 Å. In the fourth C site, C(1) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(1) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-H(1) bond length is 0.93 Å. In the fifth 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 1.51 Å. In the sixth C site, C(3) is bonded in a bent 120 degrees geometry to one C(2), one O(1), and one O(3) atom. The C(3)-O(1) bond length is 1.24 Å. The C(3)-O(3) bond length is 1.23 Å. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) 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 bent 120 degrees geometry to one Dy(1) and one C(3) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Dy(1) and one C(5) atom. In the third O site, O(3) is bonded in a linear geometry to one Dy(1) and one C(3) atom. Linkers: 4 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 4 [Dy]. The MOF has largest included sphere 6.93 A, density 1.59 g/cm3, surface area 2391.85 m2/g, accessible volume 0.33 cm3/g