TbH6(C2O)8 crystallizes in the triclinic P-1 space group. There are two inequivalent Tb sites. In the first Tb site, Tb(1) is bonded in a 8-coordinate geometry to one O(1), one O(10), one O(2), one O(3), one O(5), one O(7), one O(8), and one O(9) atom. The Tb(1)-O(1) bond length is 2.45 Å. The Tb(1)-O(10) bond length is 2.45 Å. The Tb(1)-O(2) bond length is 2.48 Å. The Tb(1)-O(3) bond length is 2.38 Å. The Tb(1)-O(5) bond length is 2.40 Å. The Tb(1)-O(7) bond length is 2.31 Å. The Tb(1)-O(8) bond length is 2.68 Å. The Tb(1)-O(9) bond length is 2.42 Å. In the second Tb site, Tb(2) is bonded in a distorted hexagonal bipyramidal geometry to two equivalent O(11), two equivalent O(4), two equivalent O(8), and two equivalent O(9) atoms. Both Tb(2)-O(11) bond lengths are 2.42 Å. Both Tb(2)-O(4) bond lengths are 2.28 Å. Both Tb(2)-O(8) bond lengths are 2.32 Å. Both Tb(2)-O(9) bond lengths are 2.57 Å. There are twenty-four inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(23), one O(1), and one O(2) atom. The C(1)-C(23) bond length is 1.50 Å. The C(1)-O(1) bond length is 1.25 Å. The C(1)-O(2) bond length is 1.27 Å. In the second C site, C(2) is bonded in a bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(2)-C(4) bond length is 1.51 Å. The C(2)-O(3) bond length is 1.24 Å. The C(2)-O(4) bond length is 1.26 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(4), one C(9), and one H(1) atom. The C(3)-C(4) bond length is 1.40 Å. The C(3)-C(9) bond length is 1.39 Å. The C(3)-H(1) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(2), one C(3), and one C(5) atom. The C(4)-C(5) bond length is 1.39 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(4), one C(7), and one H(2) atom. The C(5)-C(7) bond length is 1.38 Å. The C(5)-H(2) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(5), and one O(6) atom. The C(6)-C(7) bond length is 1.51 Å. The C(6)-O(5) bond length is 1.23 Å. The C(6)-O(6) bond length is 1.27 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(5), one C(6), and one C(8) atom. The C(7)-C(8) bond length is 1.39 Å. In the eighth C site, C(8) is bonded in a single-bond geometry to one C(7), one C(9), and one H(3) atom. The C(8)-C(9) bond length is 1.40 Å. The C(8)-H(3) bond length is 0.93 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one C(16), one C(3), and one C(8) atom. The C(9)-C(16) bond length is 1.47 Å. In the tenth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one C(11), one O(12), and one O(7) atom. The C(10)-C(11) bond length is 1.49 Å. The C(10)-O(12) bond length is 1.28 Å. The C(10)-O(7) bond length is 1.24 Å. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to one C(10), one C(12), and one C(18) atom. The C(11)-C(12) bond length is 1.39 Å. The C(11)-C(18) bond length is 1.39 Å. In the twelfth C site, C(12) is bonded in a distorted single-bond geometry to one C(11), one C(13), and one H(4) atom. The C(12)-C(13) bond length is 1.40 Å. The C(12)-H(4) bond length is 0.93 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(12), one C(15), and one C(20) atom. The C(13)-C(15) bond length is 1.50 Å. The C(13)-C(20) bond length is 1.39 Å. In the fourteenth C site, C(14) is bonded in a bent 120 degrees geometry to one C(17), one O(11), and one O(9) atom. The C(14)-C(17) bond length is 1.49 Å. The C(14)-O(11) bond length is 1.26 Å. The C(14)-O(9) bond length is 1.25 Å. In the fifteenth C site, C(15) is bonded in a distorted bent 120 degrees geometry to one C(13), one O(10), and one O(8) atom. The C(15)-O(10) bond length is 1.24 Å. The C(15)-O(8) bond length is 1.28 Å. In the sixteenth C site, C(16) is bonded in a trigonal planar geometry to one C(18), one C(20), and one C(9) atom. The C(16)-C(18) bond length is 1.39 Å. The C(16)-C(20) bond length is 1.40 Å. In the seventeenth C site, C(17) is bonded in a trigonal planar geometry to one C(14), one C(19), and one C(21) atom. The C(17)-C(19) bond length is 1.39 Å. The C(17)-C(21) bond length is 1.38 Å. In the eighteenth C site, C(18) is bonded in a distorted single-bond geometry to one C(11), one C(16), and one H(5) atom. The C(18)-H(5) bond length is 0.93 Å. In the nineteenth C site, C(19) is bonded in a distorted single-bond geometry to one C(17), one C(23), and one H(6) atom. The C(19)-C(23) bond length is 1.39 Å. The C(19)-H(6) bond length is 0.93 Å. In the twentieth C site, C(20) is bonded in a distorted single-bond geometry to one C(13), one C(16), and one H(7) atom. The C(20)-H(7) bond length is 0.93 Å. In the twenty-first C site, C(21) is bonded in a distorted single-bond geometry to one C(17), one C(22), and one H(8) atom. The C(21)-C(22) bond length is 1.39 Å. The C(21)-H(8) bond length is 0.93 Å. In the twenty-second C site, C(22) is bonded in a trigonal planar geometry to one C(21), one C(22), and one C(24) atom. The C(22)-C(22) bond length is 1.50 Å. The C(22)-C(24) bond length is 1.40 Å. In the twenty-third C site, C(23) is bonded in a trigonal planar geometry to one C(1), one C(19), and one C(24) atom. The C(23)-C(24) bond length is 1.38 Å. In the twenty-fourth C site, C(24) is bonded in a distorted single-bond geometry to one C(22), one C(23), and one H(9) atom. The C(24)-H(9) bond length is 0.93 Å. There are nine inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) 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(3) is bonded in a single-bond geometry to one C(8) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(12) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(18) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(19) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(20) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(21) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(24) atom. There are twelve inequivalent O sites. In the first O site, O(1) is bonded in a distorted L-shaped geometry to one Tb(1) and one C(1) atom. In the second O site, O(2) is bonded in a distorted L-shaped geometry to one Tb(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Tb(1) and one C(2) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Tb(2) and one C(2) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Tb(1) and one C(6) atom. In the sixth O site, O(6) is bonded in a single-bond geometry to one C(6) atom. In the seventh O site, O(7) is bonded in a distorted bent 150 degrees geometry to one Tb(1) and one C(10) atom. In the eighth O site, O(8) is bonded in a distorted bent 150 degrees geometry to one Tb(1), one Tb(2), and one C(15) atom. In the ninth O site, O(9) is bonded in a 3-coordinate geometry to one Tb(1), one Tb(2), and one C(14) atom. In the tenth O site, O(10) is bonded in a water-like geometry to one Tb(1) and one C(15) atom. In the eleventh O site, O(11) is bonded in a distorted water-like geometry to one Tb(2) and one C(14) atom. In the twelfth O site, O(12) is bonded in a single-bond geometry to one C(10) atom. Linkers: 3 [O]C(=O)c1cc(C([O])=O)cc(-c2cc(C([O])=O)cc(C([O])=O)c2)c1. Metal clusters: 1 O=[C]O[Tb]12(O[C]=O)(O[C]=O)O[C]O[Tb]34(O[C]O1)(O[C]O2)O[C]O[Tb](O[C]=O)(O[C]=O)(O[C]=O)(O[C]O3)O[C]O4. The MOF has largest included sphere 6.94 A, density 1.50 g/cm3, surface area 2895.13 m2/g, accessible volume 0.31 cm3/g