Tb(C2O)8 crystallizes in the orthorhombic Pccn space group. Tb(1) is bonded in a 9-coordinate geometry to one O(1), one O(3), one O(4), one O(5), one O(6), one O(7), one O(8), and two equivalent O(2) atoms. The Tb(1)-O(1) bond length is 2.46 Å. The Tb(1)-O(3) bond length is 2.56 Å. The Tb(1)-O(4) bond length is 2.56 Å. The Tb(1)-O(5) bond length is 2.39 Å. The Tb(1)-O(6) bond length is 2.44 Å. The Tb(1)-O(7) bond length is 2.39 Å. The Tb(1)-O(8) bond length is 2.34 Å. There is one shorter (2.36 Å) and one longer (2.47 Å) Tb(1)-O(2) bond length. There are sixteen inequivalent C sites. In the first C site, C(1) is bonded in a bent 120 degrees geometry to one C(2), one O(5), and one O(6) atom. The C(1)-C(2) bond length is 1.51 Å. The C(1)-O(5) bond length is 1.26 Å. The C(1)-O(6) bond length is 1.26 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(4) atom. The C(2)-C(3) bond length is 1.41 Å. The C(2)-C(4) bond length is 1.38 Å. In the third C site, C(3) is bonded in a bent 120 degrees geometry to one C(2) and one C(5) atom. The C(3)-C(5) bond length is 1.39 Å. In the fourth C site, C(4) is bonded in a bent 120 degrees geometry to one C(2) and one C(6) atom. The C(4)-C(6) bond length is 1.37 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(3), one C(7), and one C(8) atom. The C(5)-C(7) bond length is 1.52 Å. The C(5)-C(8) bond length is 1.37 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(4), one C(8), and one C(9) atom. The C(6)-C(8) bond length is 1.41 Å. The C(6)-C(9) bond length is 1.51 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(10), one C(11), and one C(5) atom. The C(7)-C(10) bond length is 1.40 Å. The C(7)-C(11) bond length is 1.36 Å. In the eighth C site, C(8) is bonded in a bent 120 degrees geometry to one C(5) and one C(6) atom. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(6), one O(7), and one O(8) atom. The C(9)-O(7) bond length is 1.25 Å. The C(9)-O(8) bond length is 1.25 Å. In the tenth C site, C(10) is bonded in a bent 120 degrees geometry to one C(12) and one C(7) atom. The C(10)-C(12) bond length is 1.39 Å. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to one C(13), one C(14), and one C(7) atom. The C(11)-C(13) bond length is 1.43 Å. The C(11)-C(14) bond length is 1.52 Å. In the twelfth C site, C(12) is bonded in a bent 120 degrees geometry to one C(10) and one C(15) atom. The C(12)-C(15) bond length is 1.38 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(11), one C(15), and one C(16) atom. The C(13)-C(15) bond length is 1.36 Å. The C(13)-C(16) bond length is 1.49 Å. In the fourteenth C site, C(14) is bonded in a distorted bent 120 degrees geometry to one C(11), one O(3), and one O(4) atom. The C(14)-O(3) bond length is 1.24 Å. The C(14)-O(4) bond length is 1.21 Å. In the fifteenth C site, C(15) is bonded in a bent 120 degrees geometry to one C(12) and one C(13) atom. In the sixteenth C site, C(16) is bonded in a bent 120 degrees geometry to one C(13), one O(1), and one O(2) atom. The C(16)-O(1) bond length is 1.23 Å. The C(16)-O(2) bond length is 1.30 Å. There are eight 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(16) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to two equivalent Tb(1) and one C(16) atom. In the third O site, O(3) is bonded in a single-bond geometry to one Tb(1) and one C(14) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one Tb(1) and one C(14) atom. In the fifth O site, O(5) is bonded in an L-shaped geometry to one Tb(1) and one C(1) atom. In the sixth O site, O(6) is bonded in an L-shaped geometry to one Tb(1) and one C(1) atom. In the seventh O site, O(7) is bonded in a distorted bent 120 degrees geometry to one Tb(1) and one C(9) atom. In the eighth O site, O(8) is bonded in a distorted bent 150 degrees geometry to one Tb(1) and one C(9) atom. Linkers: 8 [O]C(=O)c1[c]c(C([O])=O)[c]c(-c2[c][c][c]c(C([O])=O)c2C([O])=O)[c]1. Metal clusters: 4 [C]1O[Tb]234(O1)O[C]O[Tb]1(O[C]O1)(O[C]O2)(O[C]O3)O[C]O4.[O][C]=O.[O][C]=O. The MOF has largest included sphere 5.29 A, density 1.49 g/cm3, surface area 3012.94 m2/g, accessible volume 0.39 cm3/g