TbC9NH3O7 crystallizes in the monoclinic C2/c space group. Tb(1) is bonded in a 7-coordinate geometry to one O(1), one O(2), one O(3), one O(6), one O(7), and two equivalent O(5) atoms. The Tb(1)-O(1) bond length is 2.34 Å. The Tb(1)-O(2) bond length is 2.39 Å. The Tb(1)-O(3) bond length is 2.45 Å. The Tb(1)-O(6) bond length is 2.35 Å. The Tb(1)-O(7) bond length is 2.51 Å. There is one shorter (2.30 Å) and one longer (2.82 Å) Tb(1)-O(5) bond length. There are nine inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(8), one O(1), and one O(6) atom. The C(1)-C(8) bond length is 1.50 Å. The C(1)-O(1) bond length is 1.26 Å. The C(1)-O(6) bond length is 1.25 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(4), one C(5), and one C(7) atom. The C(2)-C(4) bond length is 1.40 Å. The C(2)-C(5) bond length is 1.43 Å. The C(2)-C(7) bond length is 1.40 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(6), one C(7), and one C(9) atom. The C(3)-C(6) bond length is 1.39 Å. The C(3)-C(7) bond length is 1.38 Å. The C(3)-C(9) bond length is 1.50 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(2), one C(8), and one H(2) atom. The C(4)-C(8) bond length is 1.39 Å. The C(4)-H(2) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a linear geometry to one C(2) and one C(5) atom. The C(5)-C(5) bond length is 1.19 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(3), one C(8), and one H(1) atom. The C(6)-C(8) bond length is 1.38 Å. The C(6)-H(1) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(2), one C(3), and one H(3) atom. The C(7)-H(3) bond length is 0.93 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(1), one C(4), and one C(6) atom. In the ninth C site, C(9) is bonded in a bent 120 degrees geometry to one C(3), one O(2), and one O(5) atom. The C(9)-O(2) bond length is 1.24 Å. The C(9)-O(5) bond length is 1.25 Å. N(1) is bonded in a trigonal planar geometry to one O(3), one O(4), and one O(7) atom. The N(1)-O(3) bond length is 1.25 Å. The N(1)-O(4) bond length is 1.23 Å. The N(1)-O(7) bond length is 1.26 Å. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(6) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. There are seven inequivalent O sites. In the first O site, O(7) is bonded in a distorted L-shaped geometry to one Tb(1) and one N(1) atom. In the second O site, O(1) is bonded in a distorted single-bond geometry to one Tb(1) and one C(1) atom. In the third O site, O(2) is bonded in a distorted water-like geometry to one Tb(1) and one C(9) atom. In the fourth O site, O(3) is bonded in a distorted single-bond geometry to one Tb(1) and one N(1) atom. In the fifth O site, O(4) is bonded in a single-bond geometry to one N(1) atom. In the sixth O site, O(5) is bonded in a 2-coordinate geometry to two equivalent Tb(1) and one C(9) atom. In the seventh O site, O(6) is bonded in a distorted bent 150 degrees geometry to one Tb(1) and one C(1) atom. Linkers: 2 [O]C(=O)c1cc(C#Cc2cc(C([O])=O)cc(C([O])=O)c2)cc(C([O])=O)c1. Metal clusters: 2 [O]N1O[Tb]234(O[C]O[Tb]5(O[C]O2)(O[C]O3)(O[C]O4)ON([O])O5)O1. RCSR code: pts. The MOF has largest included sphere 6.19 A, density 1.20 g/cm3, surface area 2995.67 m2/g, accessible volume 0.48 cm3/g