TbC24H12(NO2)3 crystallizes in the monoclinic C2/c space group. Tb(1) is bonded in a 7-coordinate geometry to one O(1), one O(3), one O(4), one O(5), one O(6), and two equivalent O(2) atoms. The Tb(1)-O(1) bond length is 2.45 Å. The Tb(1)-O(3) bond length is 2.40 Å. The Tb(1)-O(4) bond length is 2.43 Å. The Tb(1)-O(5) bond length is 2.35 Å. The Tb(1)-O(6) bond length is 2.33 Å. There is one shorter (2.32 Å) and one longer (2.80 Å) Tb(1)-O(2) bond length. There are twenty-four inequivalent C sites. In the first C site, C(1) is bonded in a distorted trigonal planar geometry to one C(23), one N(2), and one N(3) atom. The C(1)-C(23) bond length is 1.47 Å. The C(1)-N(2) bond length is 1.34 Å. The C(1)-N(3) bond length is 1.33 Å. In the second C site, C(2) is bonded in a distorted trigonal planar geometry to one C(8), one N(1), and one N(2) atom. The C(2)-C(8) bond length is 1.48 Å. The C(2)-N(1) bond length is 1.34 Å. The C(2)-N(2) bond length is 1.34 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(16), one N(1), and one N(3) atom. The C(3)-C(16) bond length is 1.49 Å. The C(3)-N(1) bond length is 1.33 Å. The C(3)-N(3) bond length is 1.34 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(9), one O(1), and one O(4) atom. The C(4)-C(9) bond length is 1.50 Å. The C(4)-O(1) bond length is 1.24 Å. The C(4)-O(4) bond length is 1.26 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(10), one C(11), and one C(6) atom. The C(5)-C(10) bond length is 1.40 Å. The C(5)-C(11) bond length is 1.37 Å. The C(5)-C(6) bond length is 1.50 Å. In the sixth C site, C(6) is bonded in a bent 120 degrees geometry to one C(5), one O(2), and one O(3) atom. The C(6)-O(2) bond length is 1.25 Å. The C(6)-O(3) bond length is 1.26 Å. In the seventh C site, C(7) is bonded in a distorted trigonal planar geometry to one C(10), one C(16), and one H(1) atom. The C(7)-C(10) bond length is 1.38 Å. The C(7)-C(16) bond length is 1.37 Å. The C(7)-H(1) bond length is 0.95 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(12), one C(18), and one C(2) atom. The C(8)-C(12) bond length is 1.37 Å. The C(8)-C(18) bond length is 1.39 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one C(15), one C(19), and one C(4) atom. The C(9)-C(15) bond length is 1.38 Å. The C(9)-C(19) bond length is 1.40 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(5), one C(7), and one H(2) atom. The C(10)-H(2) bond length is 0.95 Å. In the eleventh C site, C(11) is bonded in a distorted single-bond geometry to one C(5) and one H(3) atom. The C(11)-H(3) bond length is 0.95 Å. In the twelfth C site, C(12) is bonded in a distorted trigonal planar geometry to one C(15), one C(8), and one H(4) atom. The C(12)-C(15) bond length is 1.40 Å. The C(12)-H(4) bond length is 0.95 Å. In the thirteenth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(17), one O(5), and one O(6) atom. The C(13)-C(17) bond length is 1.51 Å. The C(13)-O(5) bond length is 1.23 Å. The C(13)-O(6) bond length is 1.26 Å. In the fourteenth C site, C(14) is bonded in a distorted single-bond geometry to one C(17), one C(21), and one H(5) atom. The C(14)-C(17) bond length is 1.39 Å. The C(14)-C(21) bond length is 1.39 Å. The C(14)-H(5) bond length is 0.95 Å. In the fifteenth C site, C(15) is bonded in a distorted single-bond geometry to one C(12), one C(9), and one H(6) atom. The C(15)-H(6) bond length is 0.95 Å. In the sixteenth C site, C(16) is bonded in a trigonal planar geometry to one C(20), one C(3), and one C(7) atom. The C(16)-C(20) bond length is 1.39 Å. In the seventeenth C site, C(17) is bonded in a trigonal planar geometry to one C(13), one C(14), and one C(22) atom. The C(17)-C(22) bond length is 1.38 Å. In the eighteenth C site, C(18) is bonded in a distorted single-bond geometry to one C(19), one C(8), and one H(7) atom. The C(18)-C(19) bond length is 1.39 Å. The C(18)-H(7) bond length is 0.95 Å. In the nineteenth C site, C(19) is bonded in a distorted trigonal planar geometry to one C(18), one C(9), and one H(8) atom. The C(19)-H(8) bond length is 0.95 Å. In the twentieth C site, C(20) is bonded in a single-bond geometry to one C(16) and one H(9) atom. The C(20)-H(9) bond length is 0.95 Å. In the twenty-first C site, C(21) is bonded in a distorted trigonal planar geometry to one C(14), one C(23), and one H(10) atom. The C(21)-C(23) bond length is 1.38 Å. The C(21)-H(10) bond length is 0.95 Å. In the twenty-second C site, C(22) is bonded in a distorted single-bond geometry to one C(17) and one H(11) atom. The C(22)-H(11) bond length is 0.95 Å. In the twenty-third C site, C(23) is bonded in a trigonal planar geometry to one C(1), one C(21), and one C(24) atom. The C(23)-C(24) bond length is 1.40 Å. In the twenty-fourth C site, C(24) is bonded in a single-bond geometry to one C(23) and one H(12) atom. The C(24)-H(12) bond length is 0.95 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a bent 120 degrees geometry to one C(2) and one C(3) atom. In the second N site, N(2) is bonded in a bent 120 degrees geometry to one C(1) and one C(2) atom. In the third N site, N(3) is bonded in a bent 120 degrees geometry to one C(1) and one C(3) atom. There are twelve 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(10) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(11) 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(14) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(15) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(18) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(19) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(20) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(21) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(22) atom. In the twelfth H site, H(12) is bonded in a single-bond geometry to one C(24) atom. There are six 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(4) atom. In the second O site, O(2) is bonded in a 2-coordinate geometry to two equivalent Tb(1) and one C(6) atom. In the third O site, O(3) is bonded in a distorted water-like geometry to one Tb(1) and one C(6) atom. In the fourth O site, O(4) is bonded in a distorted L-shaped geometry to one Tb(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a distorted bent 150 degrees geometry to one Tb(1) and one C(13) atom. In the sixth O site, O(6) is bonded in a distorted bent 150 degrees geometry to one Tb(1) and one C(13) atom. Linkers: 8 [O]C(=O)c1ccc(cc1)C1=NC(=[N]=C([N]1)c1ccc(cc1)C(=O)[O])c1ccc(cc1)C(=O)[O]. 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. RCSR code: esg. The MOF has largest included sphere 6.13 A, density 0.95 g/cm3, surface area 3721.18 m2/g, accessible volume 0.69 cm3/g