Ni3C44H32(N3O8)2 crystallizes in the monoclinic C2/c space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a square pyramidal geometry to one N(1), one N(2), one O(1), one O(3), and one O(5) atom. The Ni(1)-N(1) bond length is 2.11 Å. The Ni(1)-N(2) bond length is 2.21 Å. The Ni(1)-O(1) bond length is 2.07 Å. The Ni(1)-O(3) bond length is 2.03 Å. The Ni(1)-O(5) bond length is 2.02 Å. In the second Ni site, Ni(2) is bonded in a square co-planar geometry to two equivalent N(3) and two equivalent O(4) atoms. Both Ni(2)-N(3) bond lengths are 2.08 Å. Both Ni(2)-O(4) bond lengths are 2.07 Å. There are twenty-two inequivalent C sites. In the first C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(7) atom. The C(3)-C(2) bond length is 1.39 Å. The C(3)-C(4) bond length is 1.39 Å. The C(3)-C(7) bond length is 1.51 Å. In the second C site, C(1) is bonded in a distorted trigonal planar geometry to one C(2), one C(6), and one N(2) atom. The C(1)-C(2) bond length is 1.40 Å. The C(1)-C(6) bond length is 1.38 Å. The C(1)-N(2) bond length is 1.45 Å. In the third C site, C(2) is bonded in a distorted single-bond geometry to one C(1), one C(3), and one H(1) atom. The C(2)-H(1) bond length is 0.95 Å. In the fourth C site, C(9) is bonded in a 3-coordinate geometry to one N(2) and two equivalent H(4,5) atoms. The C(9)-N(2) bond length is 1.49 Å. Both C(9)-H(4,5) bond lengths are 0.99 Å. In the fifth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one O(3) and one O(4) atom. The C(10)-O(3) bond length is 1.26 Å. The C(10)-O(4) bond length is 1.24 Å. In the sixth C site, C(11) is bonded in a 3-coordinate geometry to one N(2) and two equivalent H(6,7) atoms. The C(11)-N(2) bond length is 1.48 Å. Both C(11)-H(6,7) bond lengths are 0.99 Å. In the seventh C site, C(12) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(12)-O(1) bond length is 1.26 Å. The C(12)-O(2) bond length is 1.24 Å. In the eighth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(8) atom. The C(13)-N(1) bond length is 1.35 Å. The C(13)-H(8) bond length is 0.95 Å. In the ninth C site, C(14) is bonded in a distorted trigonal planar geometry to one C(16), one N(1), and one H(9) atom. The C(14)-C(16) bond length is 1.38 Å. The C(14)-N(1) bond length is 1.34 Å. The C(14)-H(9) bond length is 0.95 Å. In the tenth C site, C(15) is bonded in a distorted single-bond geometry to one C(17) and one H(10) atom. The C(15)-C(17) bond length is 1.39 Å. The C(15)-H(10) bond length is 0.95 Å. In the eleventh C site, C(16) is bonded in a distorted single-bond geometry to one C(14), one C(17), and one H(11) atom. The C(16)-C(17) bond length is 1.39 Å. The C(16)-H(11) bond length is 0.95 Å. In the twelfth C site, C(17) is bonded in a trigonal planar geometry to one C(15), one C(16), and one C(18) atom. The C(17)-C(18) bond length is 1.49 Å. In the thirteenth C site, C(18) is bonded in a trigonal planar geometry to one C(17), one C(19), and one C(20) atom. The C(18)-C(19) bond length is 1.39 Å. The C(18)-C(20) bond length is 1.39 Å. In the fourteenth C site, C(19) is bonded in a distorted single-bond geometry to one C(18) and one H(12) atom. The C(19)-H(12) bond length is 0.95 Å. In the fifteenth C site, C(20) is bonded in a distorted single-bond geometry to one C(18), one C(22), and one H(13) atom. The C(20)-C(22) bond length is 1.35 Å. The C(20)-H(13) bond length is 0.95 Å. In the sixteenth C site, C(21) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(14) atom. The C(21)-N(3) bond length is 1.34 Å. The C(21)-H(14) bond length is 0.95 Å. In the seventeenth C site, C(22) is bonded in a distorted trigonal planar geometry to one C(20), one N(3), and one H(15) atom. The C(22)-N(3) bond length is 1.35 Å. The C(22)-H(15) bond length is 0.95 Å. In the eighteenth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one H(2) atom. The C(4)-C(5) bond length is 1.39 Å. The C(4)-H(2) bond length is 0.95 Å. In the nineteenth C site, C(5) is bonded in a trigonal planar geometry to one C(4), one C(6), and one C(8) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-C(8) bond length is 1.49 Å. In the twentieth C site, C(6) is bonded in a distorted single-bond geometry to one C(1), one C(5), and one H(3) atom. The C(6)-H(3) bond length is 0.95 Å. In the twenty-first C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(5), and one O(6) atom. The C(7)-O(5) bond length is 1.25 Å. The C(7)-O(6) bond length is 1.25 Å. In the twenty-second C site, C(8) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(7), and one O(8) atom. The C(8)-O(7) bond length is 1.30 Å. The C(8)-O(8) bond length is 1.22 Å. There are three inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Ni(1), one C(13), and one C(14) atom. In the second N site, N(2) is bonded in a distorted tetrahedral geometry to one Ni(1), one C(1), one C(11), and one C(9) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Ni(2), one C(21), and one C(22) atom. There are fourteen inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(2) 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(6) atom. In the fourth H site, H(4,5) is bonded in a single-bond geometry to one C(9) atom. In the fifth H site, H(6,7) is bonded in a single-bond geometry to one C(11) atom. In the sixth H site, H(8) is bonded in a single-bond geometry to one C(13) atom. In the seventh H site, H(9) is bonded in a single-bond geometry to one C(14) atom. In the eighth H site, H(10) is bonded in a single-bond geometry to one C(15) atom. In the ninth H site, H(11) is bonded in a single-bond geometry to one C(16) atom. In the tenth H site, H(12) is bonded in a single-bond geometry to one C(19) atom. In the eleventh H site, H(13) is bonded in a single-bond geometry to one C(20) atom. In the twelfth H site, H(14) is bonded in a single-bond geometry to one C(21) atom. In the thirteenth H site, H(15) is bonded in a single-bond geometry to one C(22) atom. In the fourteenth H site, H(16) is bonded in a single-bond geometry to one O(7) atom. The H(16)-O(7) bond length is 0.86 Å. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(12) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(12) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(10) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(10) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(7) atom. In the sixth O site, O(6) is bonded in a single-bond geometry to one C(7) atom. In the seventh O site, O(7) is bonded in a water-like geometry to one C(8) and one H(16) atom. In the eighth O site, O(8) is bonded in a single-bond geometry to one C(8) atom. Linkers: 4 c1cc(-c2ccncc2)ccn1 ,4 [O]C(=O)CN(CC([O])=O)c1cc(C([O])=O)cc(C(=O)O)c1. Metal clusters: 6 [Ni]. The MOF has largest included sphere 5.38 A, density 1.26 g/cm3, surface area 4176.03 m2/g, accessible volume 0.30 cm3/g