TbC3H6(NO)6 crystallizes in the monoclinic Pc space group. There are two inequivalent Tb sites. In the first Tb site, Tb(1) is bonded in a 9-coordinate geometry to one N(1), one N(12), one N(4), one N(5), one O(12), one O(6), one O(7), one O(8), and one O(9) atom. The Tb(1)-N(1) bond length is 2.57 Å. The Tb(1)-N(12) bond length is 2.51 Å. The Tb(1)-N(4) bond length is 2.49 Å. The Tb(1)-N(5) bond length is 2.67 Å. The Tb(1)-O(12) bond length is 2.42 Å. The Tb(1)-O(6) bond length is 2.30 Å. The Tb(1)-O(7) bond length is 2.44 Å. The Tb(1)-O(8) bond length is 2.95 Å. The Tb(1)-O(9) bond length is 2.33 Å. In the second Tb site, Tb(2) is bonded in a 8-coordinate geometry to one N(9), one O(1), one O(10), one O(11), one O(2), one O(3), one O(4), and one O(5) atom. The Tb(2)-N(9) bond length is 2.49 Å. The Tb(2)-O(1) bond length is 2.37 Å. The Tb(2)-O(10) bond length is 2.32 Å. The Tb(2)-O(11) bond length is 2.46 Å. The Tb(2)-O(2) bond length is 2.39 Å. The Tb(2)-O(3) bond length is 2.64 Å. The Tb(2)-O(4) bond length is 2.35 Å. The Tb(2)-O(5) bond length is 2.44 Å. There are six inequivalent C sites. In the first C site, C(1) is bonded in a distorted water-like geometry to one N(1) and one N(4) atom. The C(1)-N(1) bond length is 1.34 Å. The C(1)-N(4) bond length is 1.34 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one O(7) and one O(8) atom. The C(2)-O(7) bond length is 1.26 Å. The C(2)-O(8) bond length is 1.28 Å. In the third C site, C(3) is bonded in a distorted trigonal planar geometry to one C(4), one N(5), and one N(8) atom. The C(3)-C(4) bond length is 1.47 Å. The C(3)-N(5) bond length is 1.34 Å. The C(3)-N(8) 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(3), one O(10), and one O(9) atom. The C(4)-O(10) bond length is 1.26 Å. The C(4)-O(9) bond length is 1.27 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(6), one N(12), and one N(9) atom. The C(5)-C(6) bond length is 1.48 Å. The C(5)-N(12) bond length is 1.34 Å. The C(5)-N(9) bond length is 1.34 Å. In the sixth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(11), and one O(12) atom. The C(6)-O(11) bond length is 1.27 Å. The C(6)-O(12) bond length is 1.27 Å. There are twelve inequivalent N sites. In the first N site, N(1) is bonded in a distorted single-bond geometry to one Tb(1), one C(1), and one N(2) atom. The N(1)-N(2) bond length is 1.34 Å. In the second N site, N(2) is bonded in a distorted water-like geometry to one N(1) and one N(3) atom. The N(2)-N(3) bond length is 1.32 Å. In the third N site, N(3) is bonded in a distorted trigonal non-coplanar geometry to one N(2), one N(4), and one H(7) atom. The N(3)-N(4) bond length is 1.34 Å. The N(3)-H(7) bond length is 1.69 Å. In the fourth N site, N(4) is bonded in a distorted trigonal planar geometry to one Tb(1), one C(1), and one N(3) atom. In the fifth N site, N(5) is bonded in a distorted single-bond geometry to one Tb(1), one C(3), and one N(6) atom. The N(5)-N(6) bond length is 1.34 Å. In the sixth N site, N(6) is bonded in a 2-coordinate geometry to one N(5) and one N(7) atom. The N(6)-N(7) bond length is 1.33 Å. In the seventh N site, N(7) is bonded in a distorted trigonal planar geometry to one N(6), one N(8), and one H(11) atom. The N(7)-N(8) bond length is 1.34 Å. The N(7)-H(11) bond length is 1.73 Å. In the eighth N site, N(8) is bonded in a 3-coordinate geometry to one C(3), one N(7), and one H(10) atom. The N(8)-H(10) bond length is 1.74 Å. In the ninth N site, N(9) is bonded in a 3-coordinate geometry to one Tb(2), one C(5), and one N(10) atom. The N(9)-N(10) bond length is 1.34 Å. In the tenth N site, N(10) is bonded in a distorted trigonal planar geometry to one N(11), one N(9), and one H(12) atom. The N(10)-N(11) bond length is 1.32 Å. The N(10)-H(12) bond length is 1.65 Å. In the eleventh N site, N(11) is bonded in a water-like geometry to one N(10) and one N(12) atom. The N(11)-N(12) bond length is 1.34 Å. In the twelfth N site, N(12) is bonded in a distorted single-bond geometry to one Tb(1), one C(5), and one N(11) atom. There are twelve inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(1) atom. The H(1)-O(1) bond length is 0.99 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(1) atom. The H(2)-O(1) bond length is 1.00 Å. In the third H site, H(3) is bonded in a single-bond geometry to one O(2) atom. The H(3)-O(2) bond length is 0.98 Å. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(2) atom. The H(4)-O(2) bond length is 0.99 Å. In the fifth H site, H(5) is bonded in a single-bond geometry to one O(3) atom. The H(5)-O(3) bond length is 1.00 Å. In the sixth H site, H(6) is bonded in a single-bond geometry to one O(3) atom. The H(6)-O(3) bond length is 0.99 Å. In the seventh H site, H(7) is bonded in a distorted single-bond geometry to one N(3) and one O(4) atom. The H(7)-O(4) bond length is 1.01 Å. In the eighth H site, H(8) is bonded in a single-bond geometry to one O(4) atom. The H(8)-O(4) bond length is 0.98 Å. In the ninth H site, H(9) is bonded in a single-bond geometry to one O(5) atom. The H(9)-O(5) bond length is 0.98 Å. In the tenth H site, H(10) is bonded in a single-bond geometry to one N(8) and one O(5) atom. The H(10)-O(5) bond length is 1.01 Å. In the eleventh H site, H(11) is bonded in a single-bond geometry to one N(7) and one O(6) atom. The H(11)-O(6) bond length is 1.01 Å. In the twelfth H site, H(12) is bonded in a distorted single-bond geometry to one N(10) and one O(6) atom. The H(12)-O(6) bond length is 1.01 Å. There are twelve inequivalent O sites. In the first O site, O(1) is bonded in a distorted water-like geometry to one Tb(2), one H(1), and one H(2) atom. In the second O site, O(2) is bonded in a distorted water-like geometry to one Tb(2), one H(3), and one H(4) atom. In the third O site, O(3) is bonded in a water-like geometry to one Tb(2), one H(5), and one H(6) atom. In the fourth O site, O(4) is bonded in a distorted water-like geometry to one Tb(2), one H(7), and one H(8) atom. In the fifth O site, O(5) is bonded in a water-like geometry to one Tb(2), one H(10), and one H(9) atom. In the sixth O site, O(6) is bonded in a distorted water-like geometry to one Tb(1), one H(11), and one H(12) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Tb(1) and one C(2) atom. In the eighth O site, O(8) is bonded in a single-bond geometry to one Tb(1) and one C(2) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one Tb(1) and one C(4) atom. In the tenth O site, O(10) is bonded in a bent 120 degrees geometry to one Tb(2) and one C(4) atom. In the eleventh O site, O(11) is bonded in a distorted bent 120 degrees geometry to one Tb(2) and one C(6) atom. In the twelfth O site, O(12) is bonded in a distorted bent 120 degrees geometry to one Tb(1) and one C(6) atom. Linkers: 4 [O]C(=O)C1=NN=N[N]1. Metal clusters: 4 [Tb]. The MOF has largest included sphere 3.05 A, density 2.44 g/cm3, surface area 2513.78 m2/g, accessible volume 0.14 cm3/g