Ni3C72N6H44O13 crystallizes in the trigonal R-3c space group. The structure consists of a Ni3C72N6H44O13 framework. Ni(1) is bonded to one N(1), one O(3), two equivalent O(1), and two equivalent O(2) atoms to form corner-sharing NiNO5 octahedra. The corner-sharing octahedral tilt angles are 60°. The Ni(1)-N(1) bond length is 2.09 Å. The Ni(1)-O(3) bond length is 2.00 Å. Both Ni(1)-O(1) bond lengths are 2.06 Å. Both Ni(1)-O(2) bond lengths are 2.08 Å. There are thirteen inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.51 Å. The C(1)-O(1) bond length is 1.27 Å. The C(1)-O(2) bond length is 1.25 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(7) atom. The C(2)-C(3) bond length is 1.37 Å. The C(2)-C(7) bond length is 1.39 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2) and one H(1) atom. The C(3)-H(1) bond length is 0.95 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(5) and one H(2) atom. The C(4)-C(5) bond length is 1.37 Å. The C(4)-H(2) bond length is 0.95 Å. In the fifth 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 sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(5), one C(7), and one H(3) atom. The C(6)-C(7) bond length is 1.38 Å. The C(6)-H(3) bond length is 0.95 Å. In the seventh C site, C(7) is bonded in a distorted trigonal planar geometry to one C(2), one C(6), and one H(4) atom. The C(7)-H(4) bond length is 0.95 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(5), one C(9), and one N(2) atom. The C(8)-C(9) bond length is 1.40 Å. The C(8)-N(2) bond length is 1.35 Å. In the ninth C site, C(9) is bonded in a distorted single-bond geometry to one C(12), one C(8), and one H(5) atom. The C(9)-C(12) bond length is 1.38 Å. The C(9)-H(5) bond length is 0.95 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(13) and one H(6) atom. The C(10)-C(13) bond length is 1.38 Å. The C(10)-H(6) bond length is 0.95 Å. In the eleventh C site, C(11) is bonded in a 2-coordinate geometry to one N(1) and one H(7) atom. The C(11)-N(1) bond length is 1.33 Å. The C(11)-H(7) bond length is 0.95 Å. In the twelfth C site, C(12) is bonded in a trigonal planar geometry to one C(13) and two equivalent C(9) atoms. The C(12)-C(13) bond length is 1.50 Å. In the thirteenth C site, C(13) is bonded in a trigonal planar geometry to one C(12) and two equivalent C(10) atoms. There are two inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Ni(1) and two equivalent C(11) atoms. In the second N site, N(2) is bonded in a bent 120 degrees geometry to two equivalent C(8) atoms. There are eight inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) 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) is bonded in a single-bond geometry to one C(7) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(9) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(10) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(11) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one O(3) atom. The H(8)-O(3) bond length is 1.00 Å. There are three inequivalent O sites. In the first O site, O(3) is bonded in a linear geometry to three equivalent Ni(1) and two equivalent H(8) atoms. In the second O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(1) atom. In the third O site, O(2) is bonded in a distorted bent 150 degrees geometry to one Ni(1) and one C(1) atom. Linkers: 19 [O]C(=O)c1ccc(-c2cc(-c3ccncc3)cc(-c3ccc(C([O])=O)cc3)n2)cc1. Metal clusters: 6 O.[C]1O[Ni]23O[C]O[Ni]4(O1)O[C]O[Ni](O[C]O2)(O[C]O3)O[C]O4. RCSR code: pcu. The MOF has largest included sphere 6.75 A, density 0.80 g/cm3, surface area 4356.62 m2/g, accessible volume 0.84 cm3/g