Yb2H2(C5O4)3 crystallizes in the monoclinic C2/m space group. Yb(1) is bonded in a 6-coordinate geometry to one O(1), one O(2), one O(3), one O(4), one O(5), and one O(6) atom. The Yb(1)-O(1) bond length is 2.39 Å. The Yb(1)-O(2) bond length is 2.37 Å. The Yb(1)-O(3) bond length is 2.22 Å. The Yb(1)-O(4) bond length is 2.27 Å. The Yb(1)-O(5) bond length is 2.42 Å. The Yb(1)-O(6) bond length is 2.32 Å. There are nine inequivalent C sites. In the first C site, C(7) is bonded in a distorted single-bond geometry to two equivalent C(1) and one H(1) atom. Both C(7)-C(1) bond lengths are 1.39 Å. The C(7)-H(1) bond length is 0.93 Å. In the second C site, C(8) is bonded in a distorted single-bond geometry to two equivalent C(2) and one H(2) atom. Both C(8)-C(2) bond lengths are 1.41 Å. The C(8)-H(2) bond length is 0.93 Å. In the third C site, C(9) is bonded in a bent 120 degrees geometry to two equivalent C(6) atoms. Both C(9)-C(6) bond lengths are 1.39 Å. In the fourth C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(3), and one C(7) atom. The C(1)-C(2) bond length is 1.37 Å. The C(1)-C(3) bond length is 1.51 Å. In the fifth C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(4), and one C(8) atom. The C(2)-C(4) bond length is 1.52 Å. In the sixth C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(1), and one O(2) atom. The C(3)-O(1) bond length is 1.26 Å. The C(3)-O(2) bond length is 1.27 Å. In the seventh C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(3), and one O(4) atom. The C(4)-O(3) bond length is 1.26 Å. The C(4)-O(4) bond length is 1.23 Å. In the eighth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(6), one O(5), and one O(6) atom. The C(5)-C(6) bond length is 1.50 Å. The C(5)-O(5) bond length is 1.28 Å. The C(5)-O(6) bond length is 1.25 Å. In the ninth C site, C(6) is bonded in a trigonal planar geometry to one C(5), one C(6), and one C(9) atom. The C(6)-C(6) bond length is 1.41 Å. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(7) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(8) atom. There are six inequivalent O sites. In the first O site, O(1) is bonded in a distorted L-shaped geometry to one Yb(1) and one C(3) atom. In the second O site, O(2) is bonded in a distorted L-shaped geometry to one Yb(1) and one C(3) atom. In the third O site, O(3) is bonded in a linear geometry to one Yb(1) and one C(4) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one Yb(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a distorted L-shaped geometry to one Yb(1) and one C(5) atom. In the sixth O site, O(6) is bonded in a distorted single-bond geometry to one Yb(1) and one C(5) atom. Linkers: 1 [O]C(=O)c1[c]c(C([O])=O)c(C([O])=O)[c]c1C([O])=O ,2 [O]C(=O)c1cc(C([O])=O)c(C([O])=O)cc1C([O])=O. Metal clusters: 2 [C]1O[Yb]23(O1)(O[C]O2)O[C]O[Yb]12(O[C]O1)(O[C]O2)O[C]O3. RCSR code: fsy. The MOF has largest included sphere 4.17 A, density 2.28 g/cm3, surface area 2312.63 m2/g, accessible volume 0.19 cm3/g