Ni3C18H6O13 crystallizes in the orthorhombic Imm2 space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(4) and four equivalent O(1) atoms to form distorted corner-sharing NiO5 square pyramids. The Ni(1)-O(4) bond length is 1.94 Å. All Ni(1)-O(1) bond lengths are 2.07 Å. In the second Ni site, Ni(2) is bonded to one O(4), two equivalent O(2), and two equivalent O(3) atoms to form corner-sharing NiO5 square pyramids. The Ni(2)-O(4) bond length is 1.96 Å. Both Ni(2)-O(2) bond lengths are 2.02 Å. Both Ni(2)-O(3) bond lengths are 2.01 Å. There are six inequivalent C sites. In the first C site, C(6) is bonded in a bent 120 degrees geometry to one C(5) and two equivalent O(3) atoms. The C(6)-C(5) bond length is 1.50 Å. Both C(6)-O(3) bond lengths are 1.24 Å. In the second C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(3), and one C(4) atom. The C(1)-C(2) bond length is 1.37 Å. The C(1)-C(3) bond length is 1.51 Å. The C(1)-C(4) bond length is 1.37 Å. In the third C site, C(2) is bonded in a distorted single-bond geometry to one C(1), one C(5), and one H(1) atom. The C(2)-C(5) bond length is 1.37 Å. The C(2)-H(1) bond length is 0.95 Å. In the fourth C site, C(3) is bonded in a distorted trigonal planar geometry to one C(1), one O(1), and one O(2) atom. The C(3)-O(1) bond length is 1.23 Å. The C(3)-O(2) bond length is 1.24 Å. In the fifth C site, C(4) is bonded in a single-bond geometry to two equivalent C(1) and one H(2) atom. The C(4)-H(2) bond length is 0.95 Å. In the sixth C site, C(5) is bonded in a trigonal planar geometry to one C(6) and two equivalent C(2) atoms. There are two 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. There are four inequivalent O sites. In the first O site, O(4) is bonded in a trigonal planar geometry to one Ni(1) and two equivalent Ni(2) atoms. In the second O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(3) atom. In the third O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(3) atom. In the fourth O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(6) atom. Linkers: 4 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 2 [C]1O[Ni]23O[C]O[Ni]45(O1)O[C]O[Ni](O[C]O2)(O[C]O3)(O[C]O4)O5. RCSR code: sit. The MOF has largest included sphere 7.01 A, density 1.11 g/cm3, surface area 3307.82 m2/g, accessible volume 0.52 cm3/g