LiTbH8(C2O)8 crystallizes in the triclinic P-1 space group. Li(1) is bonded in a distorted rectangular see-saw-like geometry to one O(1), one O(2), one O(5), and one O(6) atom. The Li(1)-O(1) bond length is 1.99 Å. The Li(1)-O(2) bond length is 1.99 Å. The Li(1)-O(5) bond length is 1.89 Å. The Li(1)-O(6) bond length is 1.89 Å. Tb(1) is bonded in a 8-coordinate geometry to one O(1), one O(2), one O(3), one O(4), one O(5), one O(6), one O(7), and one O(8) atom. The Tb(1)-O(1) bond length is 2.39 Å. The Tb(1)-O(2) bond length is 2.39 Å. The Tb(1)-O(3) bond length is 2.28 Å. The Tb(1)-O(4) bond length is 2.28 Å. The Tb(1)-O(5) bond length is 2.40 Å. The Tb(1)-O(6) bond length is 2.40 Å. The Tb(1)-O(7) bond length is 2.45 Å. The Tb(1)-O(8) bond length is 2.45 Å. There are thirteen inequivalent C sites. In the first C site, C(1,2) is bonded in a distorted trigonal planar geometry to one C(1,2); one C(7); and one H(1,2) atom. The C(1,2)-C(1,2) bond length is 1.39 Å. The C(1,2)-C(7) bond length is 1.40 Å. The C(1,2)-H(1,2) bond length is 1.09 Å. In the second C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(1), and one O(3) atom. The C(3)-C(7) bond length is 1.49 Å. The C(3)-O(1) bond length is 1.29 Å. The C(3)-O(3) bond length is 1.27 Å. In the third C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(8), one O(2), and one O(4) atom. The C(4)-C(8) bond length is 1.49 Å. The C(4)-O(2) bond length is 1.29 Å. The C(4)-O(4) bond length is 1.27 Å. In the fourth C site, C(5,6) is bonded in a distorted single-bond geometry to one C(7) and one H(3,4) atom. The C(5,6)-C(7) bond length is 1.40 Å. The C(5,6)-H(3,4) bond length is 1.09 Å. In the fifth C site, C(7) is bonded in a trigonal planar geometry to one C(1,2); one C(3); and one C(5,6) atom. In the sixth C site, C(8) is bonded in a trigonal planar geometry to one C(1,2); one C(4); and one C(5,6) atom. The C(8)-C(1,2) bond length is 1.40 Å. The C(8)-C(5,6) bond length is 1.40 Å. In the seventh C site, C(9,10) is bonded in a trigonal planar geometry to one C(11), one C(13), and one C(15) atom. The C(9,10)-C(11) bond length is 1.49 Å. The C(9,10)-C(13) bond length is 1.40 Å. The C(9,10)-C(15) bond length is 1.40 Å. In the eighth C site, C(11) is bonded in a bent 120 degrees geometry to one C(9,10); one O(5); and one O(7) atom. The C(11)-O(5) bond length is 1.29 Å. The C(11)-O(7) bond length is 1.27 Å. In the ninth C site, C(12) is bonded in a bent 120 degrees geometry to one C(9,10); one O(6); and one O(8) atom. The C(12)-C(9,10) bond length is 1.49 Å. The C(12)-O(6) bond length is 1.29 Å. The C(12)-O(8) bond length is 1.27 Å. In the tenth C site, C(13) is bonded in a distorted trigonal planar geometry to one C(15); one C(9,10); and one H(5,6) atom. The C(13)-C(15) bond length is 1.39 Å. The C(13)-H(5,6) bond length is 1.09 Å. In the eleventh C site, C(14) is bonded in a distorted trigonal planar geometry to one C(16); one C(9,10); and one H(5,6) atom. The C(14)-C(16) bond length is 1.39 Å. The C(14)-C(9,10) bond length is 1.40 Å. The C(14)-H(5,6) bond length is 1.09 Å. In the twelfth C site, C(15) is bonded in a distorted single-bond geometry to one C(13); one C(9,10); and one H(7,8) atom. The C(15)-H(7,8) bond length is 1.09 Å. In the thirteenth C site, C(16) is bonded in a distorted single-bond geometry to one C(14); one C(9,10); and one H(7,8) atom. The C(16)-C(9,10) bond length is 1.40 Å. The C(16)-H(7,8) bond length is 1.09 Å. There are four inequivalent H sites. In the first H site, H(1,2) is bonded in a single-bond geometry to one C(1,2) atom. In the second H site, H(3,4) is bonded in a single-bond geometry to one C(5,6) atom. In the third H site, H(5,6) is bonded in a single-bond geometry to one C(13) atom. In the fourth H site, H(7,8) is bonded in a single-bond geometry to one C(15) atom. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a distorted trigonal planar geometry to one Li(1), one Tb(1), and one C(3) atom. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to one Li(1), one Tb(1), and one C(4) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Tb(1) and one C(3) atom. In the fourth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Tb(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a 3-coordinate geometry to one Li(1), one Tb(1), and one C(11) atom. In the sixth O site, O(6) is bonded in a 3-coordinate geometry to one Li(1), one Tb(1), and one C(12) atom. In the seventh O site, O(7) is bonded in a distorted L-shaped geometry to one Tb(1) and one C(11) atom. In the eighth O site, O(8) is bonded in a distorted L-shaped geometry to one Tb(1) and one C(12) atom. Linkers: 4 [O]C(=O)c1ccc(C([O])=O)cc1. Metal clusters: 2 [Li] ,2 [Tb]. The MOF has largest included sphere 3.12 A, density 1.98 g/cm3, surface area 2826.63 m2/g, accessible volume 0.13 cm3/g