Ni3C30H26(N6O7)2 crystallizes in the monoclinic P2_1/c space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one N(1), one N(6), one O(1), one O(2), one O(4), and one O(6) atom to form corner-sharing NiN2O4 octahedra. The corner-sharing octahedral tilt angles are 72°. The Ni(1)-N(1) bond length is 2.06 Å. The Ni(1)-N(6) bond length is 2.07 Å. The Ni(1)-O(1) bond length is 2.14 Å. The Ni(1)-O(2) bond length is 2.06 Å. The Ni(1)-O(4) bond length is 2.00 Å. The Ni(1)-O(6) bond length is 2.07 Å. In the second Ni site, Ni(2) is bonded to two equivalent N(2), two equivalent N(5), and two equivalent O(1) atoms to form corner-sharing NiN4O2 octahedra. The corner-sharing octahedral tilt angles are 72°. Both Ni(2)-N(2) bond lengths are 2.09 Å. Both Ni(2)-N(5) bond lengths are 2.08 Å. Both Ni(2)-O(1) bond lengths are 2.06 Å. There are fifteen inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one N(1), one N(3), and one H(3) atom. The C(1)-N(1) bond length is 1.30 Å. The C(1)-N(3) bond length is 1.36 Å. The C(1)-H(3) bond length is 0.94 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one N(2), one N(3), and one H(4) atom. The C(2)-N(2) bond length is 1.30 Å. The C(2)-N(3) bond length is 1.35 Å. The C(2)-H(4) bond length is 0.94 Å. In the third C site, C(3) is bonded in a 3-coordinate geometry to one N(3) and two equivalent H(5,6) atoms. The C(3)-N(3) bond length is 1.47 Å. Both C(3)-H(5,6) bond lengths are 0.98 Å. In the fourth C site, C(4) is bonded in a 3-coordinate geometry to one N(4) and two equivalent H(7,8) atoms. The C(4)-N(4) bond length is 1.47 Å. Both C(4)-H(7,8) bond lengths are 0.98 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one N(4), one N(5), and one H(9) atom. The C(5)-N(4) bond length is 1.35 Å. The C(5)-N(5) bond length is 1.31 Å. The C(5)-H(9) bond length is 0.94 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one N(4), one N(6), and one H(10) atom. The C(6)-N(4) bond length is 1.35 Å. The C(6)-N(6) bond length is 1.30 Å. The C(6)-H(10) bond length is 0.94 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(12), one C(13), and one C(8) atom. The C(7)-C(12) bond length is 1.39 Å. The C(7)-C(13) bond length is 1.51 Å. The C(7)-C(8) bond length is 1.40 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(7), one C(9), and one H(11) atom. The C(8)-C(9) bond length is 1.39 Å. The C(8)-H(11) bond length is 0.94 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one C(10), one C(14), and one C(8) atom. The C(9)-C(10) bond length is 1.39 Å. The C(9)-C(14) bond length is 1.51 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(11), one C(9), and one H(12) atom. The C(10)-C(11) bond length is 1.39 Å. The C(10)-H(12) bond length is 0.94 Å. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to one C(10), one C(12), and one C(15) atom. The C(11)-C(12) bond length is 1.39 Å. The C(11)-C(15) bond length is 1.49 Å. In the twelfth C site, C(12) is bonded in a distorted single-bond geometry to one C(11), one C(7), and one H(13) atom. The C(12)-H(13) bond length is 0.94 Å. In the thirteenth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(2), and one O(3) atom. The C(13)-O(2) bond length is 1.25 Å. The C(13)-O(3) bond length is 1.27 Å. In the fourteenth C site, C(14) is bonded in a distorted bent 120 degrees geometry to one C(9), one O(4), and one O(5) atom. The C(14)-O(4) bond length is 1.26 Å. The C(14)-O(5) bond length is 1.24 Å. In the fifteenth C site, C(15) is bonded in a distorted bent 120 degrees geometry to one C(11), one O(6), and one O(7) atom. The C(15)-O(6) bond length is 1.26 Å. The C(15)-O(7) bond length is 1.27 Å. There are six inequivalent N sites. In the first N site, N(1) is bonded in a 3-coordinate geometry to one Ni(1), one C(1), and one N(2) atom. The N(1)-N(2) bond length is 1.38 Å. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one Ni(2), one C(2), and one N(1) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one C(1), one C(2), and one C(3) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one C(4), one C(5), and one C(6) atom. In the fifth N site, N(5) is bonded in a distorted trigonal planar geometry to one Ni(2), one C(5), and one N(6) atom. The N(5)-N(6) bond length is 1.38 Å. In the sixth N site, N(6) is bonded in a 3-coordinate geometry to one Ni(1), one C(6), and one N(5) atom. There are eleven inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(1) and one O(3) atom. The H(1)-O(1) bond length is 0.94 Å. The H(1)-O(3) bond length is 1.61 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(1) and one O(7) atom. The H(2)-O(1) bond length is 0.86 Å. The H(2)-O(7) bond length is 1.69 Å. In the third H site, H(3) is bonded in a single-bond geometry to one C(1) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(2) atom. In the fifth H site, H(5,6) is bonded in a single-bond geometry to one C(3) atom. In the sixth H site, H(7,8) is bonded in a single-bond geometry to one C(4) atom. In the seventh H site, H(9) is bonded in a single-bond geometry to one C(5) atom. In the eighth H site, H(10) is bonded in a single-bond geometry to one C(6) atom. In the ninth H site, H(11) is bonded in a single-bond geometry to one C(8) atom. In the tenth H site, H(12) is bonded in a single-bond geometry to one C(10) atom. In the eleventh H site, H(13) is bonded in a single-bond geometry to one C(12) atom. There are seven inequivalent O sites. In the first O site, O(1) is bonded in a distorted water-like geometry to one Ni(1), one Ni(2), one H(1), and one H(2) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(13) atom. In the third O site, O(3) is bonded in a water-like geometry to one C(13) and one H(1) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(14) atom. In the fifth O site, O(5) is bonded in a single-bond geometry to one C(14) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(15) atom. In the seventh O site, O(7) is bonded in a distorted single-bond geometry to one C(15) and one H(2) atom. Linkers: 4 c1nncn1CCn1cnnc1 ,4 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 2 O.O.O=[C]O[Ni]1(O[C]=O)(O[C]=O)[N]N=[Ni]2(N=N1)N=N[Ni](O[C]=O)(O[C]=O)(O[C]=O)N=N2. The MOF has largest included sphere 7.01 A, density 1.02 g/cm3, surface area 3979.31 m2/g, accessible volume 0.53 cm3/g