DyH3(C3O2)3 crystallizes in the tetragonal P4_322 space group. Dy(1) is bonded in a 6-coordinate geometry to two equivalent O(1), two equivalent O(2), and two equivalent O(3) atoms. Both Dy(1)-O(1) bond lengths are 2.33 Å. Both Dy(1)-O(2) bond lengths are 2.26 Å. Both Dy(1)-O(3) bond lengths are 2.25 Å. There are six inequivalent C sites. In the first C site, C(3) is bonded in a trigonal planar geometry to one C(6) and two equivalent C(4) atoms. The C(3)-C(6) bond length is 1.50 Å. Both C(3)-C(4) bond lengths are 1.40 Å. In the second C site, C(4) is bonded in a distorted trigonal planar geometry to one C(2), one C(3), and one H(1) atom. The C(4)-C(2) bond length is 1.40 Å. The C(4)-H(1) bond length is 1.09 Å. In the third C site, C(5) is bonded in a single-bond geometry to two equivalent C(2) and one H(2) atom. Both C(5)-C(2) bond lengths are 1.40 Å. The C(5)-H(2) bond length is 1.09 Å. In the fourth C site, C(1) is bonded in a bent 120 degrees geometry to one C(2), one O(1), and one O(3) atom. The C(1)-C(2) bond length is 1.49 Å. The C(1)-O(1) bond length is 1.27 Å. The C(1)-O(3) bond length is 1.28 Å. In the fifth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(3) and two equivalent O(2) atoms. Both C(6)-O(2) bond lengths are 1.27 Å. In the sixth C site, C(2) is bonded in a trigonal planar geometry to one C(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(4) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(5) atom. There are three inequivalent O sites. In the first O site, O(3) is bonded in a linear geometry to one Dy(1) and one C(1) atom. In the second O site, O(1) is bonded in a bent 120 degrees geometry to one Dy(1) and one C(1) atom. In the third O site, O(2) is bonded in a bent 150 degrees geometry to one Dy(1) and one C(6) 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 6.95 A, density 1.63 g/cm3, surface area 2321.51 m2/g, accessible volume 0.31 cm3/g