Ni3H16(C16O9)2(C7H4)4 is Indium-derived structured and crystallizes in the orthorhombic Pmna space group. The structure is zero-dimensional and consists of four C7H4 clusters and two Ni3H16(C16O9)2 clusters. In each C7H4 cluster, there are eight inequivalent C sites. In the first C site, C(2) is bonded in a trigonal planar geometry to one C(15), one C(5), and one C(7) atom. The C(2)-C(15) bond length is 1.49 Å. The C(2)-C(5) bond length is 1.38 Å. The C(2)-C(7) bond length is 1.39 Å. In the second C site, C(3) is bonded in a trigonal planar geometry to one C(10), one C(16), and one C(9) atom. The C(3)-C(10) bond length is 1.37 Å. The C(3)-C(16) bond length is 1.50 Å. The C(3)-C(9) bond length is 1.36 Å. In the third C site, C(5) is bonded in a distorted single-bond geometry to one C(2) and one H(1) atom. The C(5)-H(1) bond length is 0.96 Å. In the fourth C site, C(7) is bonded in a distorted single-bond geometry to one C(2) and one H(3) atom. The C(7)-H(3) bond length is 0.96 Å. In the fifth C site, C(9) is bonded in a distorted single-bond geometry to one C(3) and one H(5) atom. The C(9)-H(5) bond length is 0.96 Å. In the sixth C site, C(10) is bonded in a distorted single-bond geometry to one C(3) and one H(6) atom. The C(10)-H(6) bond length is 0.96 Å. In the seventh C site, C(15) is bonded in a trigonal planar geometry to one C(16) and two equivalent C(2) atoms. The C(15)-C(16) bond length is 1.35 Å. In the eighth C site, C(16) is bonded in a trigonal planar geometry to one C(15) and two equivalent C(3) atoms. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(5) atom. In the second H site, H(3) is bonded in a single-bond geometry to one C(7) atom. In the third H site, H(5) is bonded in a single-bond geometry to one C(9) atom. In the fourth H site, H(6) is bonded in a single-bond geometry to one C(10) atom. In each Ni3H16(C16O9)2 cluster, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(5), two equivalent O(1), and two equivalent O(3) atoms to form corner-sharing NiO5 square pyramids. The corner-sharing octahedral tilt angles are 63°. The Ni(1)-O(5) bond length is 2.07 Å. Both Ni(1)-O(1) bond lengths are 2.04 Å. Both Ni(1)-O(3) bond lengths are 2.08 Å. In the second Ni site, Ni(2) is bonded to two equivalent O(5) and four equivalent O(2) atoms to form corner-sharing NiO6 octahedra. Both Ni(2)-O(5) bond lengths are 2.05 Å. All Ni(2)-O(2) bond lengths are 1.99 Å. There are eight inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(1), and one O(2) atom. The C(1)-C(4) bond length is 1.51 Å. The C(1)-O(1) bond length is 1.25 Å. The C(1)-O(2) bond length is 1.24 Å. In the second C site, C(4) is bonded in a trigonal planar geometry to one C(1), one C(6), and one C(8) atom. The C(4)-C(6) bond length is 1.38 Å. The C(4)-C(8) bond length is 1.37 Å. In the third C site, C(6) is bonded in a distorted single-bond geometry to one C(4) and one H(2) atom. The C(6)-H(2) bond length is 0.96 Å. In the fourth C site, C(8) is bonded in a distorted single-bond geometry to one C(4) and one H(4) atom. The C(8)-H(4) bond length is 0.96 Å. In the fifth C site, C(11) is bonded in a distorted single-bond geometry to one C(12) and one H(7) atom. The C(11)-C(12) bond length is 1.37 Å. The C(11)-H(7) bond length is 0.96 Å. In the sixth C site, C(12) is bonded in a trigonal planar geometry to one C(11), one C(13), and one C(14) atom. The C(12)-C(13) bond length is 1.51 Å. The C(12)-C(14) bond length is 1.36 Å. In the seventh C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(12), one O(3), and one O(4) atom. The C(13)-O(3) bond length is 1.25 Å. The C(13)-O(4) bond length is 1.25 Å. In the eighth C site, C(14) is bonded in a distorted single-bond geometry to one C(12) and one H(8) atom. The C(14)-H(8) bond length is 0.96 Å. There are four inequivalent H sites. In the first H site, H(2) is bonded in a single-bond geometry to one C(6) atom. In the second H site, H(4) is bonded in a single-bond geometry to one C(8) atom. In the third H site, H(7) is bonded in a single-bond geometry to one C(11) atom. In the fourth H site, H(8) is bonded in a single-bond geometry to one C(14) atom. There are five 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(1) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Ni(2) and one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(13) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(13) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Ni(1) and one Ni(2) atom. Linkers: 4 [O]C(=O)c1ccc(C(=C(c2ccc(C([O])=O)cc2)c2ccc(C([O])=O)cc2)c2ccc(C([O])=O)cc2)cc1. Metal clusters: 2 O=[C]O[Ni]12(O[C]=O)O[C]O[Ni]34(O[C]O1)(O[C]O[Ni](O[C]=O)(O[C]=O)(O[C]O3)O4)O2. RCSR code: scu. The MOF has largest included sphere 6.85 A, density 0.92 g/cm3, surface area 4401.70 m2/g, accessible volume 0.66 cm3/g