TmCoC16H16(N5O3)2 crystallizes in the triclinic P-1 space group. Tm(1) is bonded in a 8-coordinate geometry to one N(3), one N(4), one O(1), one O(2), one O(3), one O(4), one O(5), and one O(6) atom. The Tm(1)-N(3) bond length is 2.38 Å. The Tm(1)-N(4) bond length is 2.41 Å. The Tm(1)-O(1) bond length is 2.32 Å. The Tm(1)-O(2) bond length is 2.29 Å. The Tm(1)-O(3) bond length is 2.26 Å. The Tm(1)-O(4) bond length is 2.32 Å. The Tm(1)-O(5) bond length is 2.34 Å. The Tm(1)-O(6) bond length is 2.44 Å. Co(1) is bonded in an octahedral geometry to one C(1), one C(2), one C(3), one C(5), one C(7), and one C(8) atom. The Co(1)-C(1) bond length is 1.86 Å. The Co(1)-C(2) bond length is 1.86 Å. The Co(1)-C(3) bond length is 1.87 Å. The Co(1)-C(5) bond length is 1.86 Å. The Co(1)-C(7) bond length is 1.87 Å. The Co(1)-C(8) bond length is 1.87 Å. There are sixteen inequivalent C sites. In the first C site, C(1) is bonded in a linear geometry to one Co(1) and one N(3) atom. The C(1)-N(3) bond length is 1.17 Å. In the second C site, C(2) is bonded in a linear geometry to one Co(1) and one N(4) atom. The C(2)-N(4) bond length is 1.17 Å. In the third C site, C(3) is bonded in a linear geometry to one Co(1) and one N(9) atom. The C(3)-N(9) bond length is 1.17 Å. In the fourth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(13), one N(1), and one H(4) atom. The C(4)-C(13) bond length is 1.38 Å. The C(4)-N(1) bond length is 1.36 Å. The C(4)-H(4) bond length is 1.08 Å. In the fifth C site, C(5) is bonded in a linear geometry to one Co(1) and one N(7) atom. The C(5)-N(7) bond length is 1.18 Å. In the sixth C site, C(6) is bonded in a distorted trigonal planar geometry to one C(9), one N(2), and one H(6) atom. The C(6)-C(9) bond length is 1.38 Å. The C(6)-N(2) bond length is 1.36 Å. The C(6)-H(6) bond length is 1.08 Å. In the seventh C site, C(7) is bonded in a linear geometry to one Co(1) and one N(8) atom. The C(7)-N(8) bond length is 1.17 Å. In the eighth C site, C(8) is bonded in a linear geometry to one Co(1) and one N(6) atom. The C(8)-N(6) bond length is 1.17 Å. In the ninth C site, C(9) is bonded in a distorted single-bond geometry to one C(11), one C(6), and one H(1) atom. The C(9)-C(11) bond length is 1.40 Å. The C(9)-H(1) bond length is 1.09 Å. In the tenth C site, C(10) is bonded in a distorted trigonal planar geometry to one C(13), one C(14), and one N(10) atom. The C(10)-C(13) bond length is 1.40 Å. The C(10)-C(14) bond length is 1.41 Å. The C(10)-N(10) bond length is 1.41 Å. In the eleventh C site, C(11) is bonded in a distorted trigonal planar geometry to one C(16), one C(9), and one N(5) atom. The C(11)-C(16) bond length is 1.41 Å. The C(11)-N(5) bond length is 1.40 Å. In the twelfth C site, C(12) is bonded in a distorted trigonal planar geometry to one C(14), one N(1), and one H(3) atom. The C(12)-C(14) bond length is 1.38 Å. The C(12)-N(1) bond length is 1.37 Å. The C(12)-H(3) bond length is 1.09 Å. In the thirteenth C site, C(13) is bonded in a distorted single-bond geometry to one C(10), one C(4), and one H(2) atom. The C(13)-H(2) bond length is 1.09 Å. In the fourteenth C site, C(14) is bonded in a distorted trigonal planar geometry to one C(10), one C(12), and one H(7) atom. The C(14)-H(7) bond length is 1.09 Å. In the fifteenth C site, C(15) is bonded in a distorted trigonal planar geometry to one C(16), one N(2), and one H(5) atom. The C(15)-C(16) bond length is 1.37 Å. The C(15)-N(2) bond length is 1.37 Å. The C(15)-H(5) bond length is 1.08 Å. In the sixteenth C site, C(16) is bonded in a distorted trigonal planar geometry to one C(11), one C(15), and one H(8) atom. The C(16)-H(8) bond length is 1.09 Å. There are ten inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one C(12), one C(4), and one O(2) atom. The N(1)-O(2) bond length is 1.32 Å. In the second N site, N(2) is bonded in a trigonal planar geometry to one C(15), one C(6), and one O(3) atom. The N(2)-O(3) bond length is 1.31 Å. In the third N site, N(3) is bonded in a distorted linear geometry to one Tm(1) and one C(1) atom. In the fourth N site, N(4) is bonded in a distorted linear geometry to one Tm(1) and one C(2) atom. In the fifth N site, N(5) is bonded in a distorted bent 120 degrees geometry to one C(11) and one N(5) atom. The N(5)-N(5) bond length is 1.28 Å. In the sixth N site, N(6) is bonded in a linear geometry to one C(8) and one H(16) atom. The N(6)-H(16) bond length is 1.66 Å. In the seventh N site, N(7) is bonded in a single-bond geometry to one C(5) atom. In the eighth N site, N(8) is bonded in a bent 150 degrees geometry to one C(7) and one H(12) atom. The N(8)-H(12) bond length is 1.65 Å. In the ninth N site, N(9) is bonded in a distorted bent 150 degrees geometry to one C(3) and one H(10) atom. The N(9)-H(10) bond length is 1.68 Å. In the tenth N site, N(10) is bonded in a distorted bent 120 degrees geometry to one C(10) and one N(10) atom. The N(10)-N(10) bond length is 1.27 Å. There are sixteen inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(9) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(13) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(12) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(4) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(15) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(6) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(14) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(16) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one O(1) atom. The H(9)-O(1) bond length is 0.99 Å. In the tenth H site, H(10) is bonded in a single-bond geometry to one N(9) and one O(1) atom. The H(10)-O(1) bond length is 1.01 Å. In the eleventh H site, H(11) is bonded in a single-bond geometry to one O(4) atom. The H(11)-O(4) bond length is 0.97 Å. In the twelfth H site, H(12) is bonded in a distorted linear geometry to one N(8) and one O(4) atom. The H(12)-O(4) bond length is 1.01 Å. In the thirteenth H site, H(13) is bonded in a single-bond geometry to one O(6) atom. The H(13)-O(6) bond length is 0.99 Å. In the fourteenth H site, H(14) is bonded in a single-bond geometry to one O(6) atom. The H(14)-O(6) bond length is 0.97 Å. In the fifteenth H site, H(15) is bonded in a single-bond geometry to one O(5) atom. The H(15)-O(5) bond length is 0.97 Å. In the sixteenth H site, H(16) is bonded in a distorted single-bond geometry to one N(6) and one O(5) atom. The H(16)-O(5) bond length is 1.01 Å. There are six inequivalent O sites. In the first O site, O(1) is bonded in a water-like geometry to one Tm(1), one H(10), and one H(9) atom. In the second O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Tm(1) and one N(1) atom. In the third O site, O(3) is bonded in a bent 150 degrees geometry to one Tm(1) and one N(2) atom. In the fourth O site, O(4) is bonded in a distorted water-like geometry to one Tm(1), one H(11), and one H(12) atom. In the fifth O site, O(5) is bonded in a distorted water-like geometry to one Tm(1), one H(15), and one H(16) atom. In the sixth O site, O(6) is bonded in a water-like geometry to one Tm(1), one H(13), and one H(14) atom. Linkers: 2 [O-][n+]1ccc([N][N]c2cc[n+]([O-])cc2)cc1. Metal clusters: 2 [Tm] ,2 [Co]. The MOF has largest included sphere 3.14 A, density 1.90 g/cm3, surface area 3557.36 m2/g, accessible volume 0.14 cm3/g