Ni3C36H12O13(CH)12 crystallizes in the trigonal P-31c space group. The structure consists of twenty-four 02329_fluka molecules inside a Ni3C36H12O13 framework. In the Ni3C36H12O13 framework, Ni(1) is bonded to one O(3), two equivalent O(1), and two equivalent O(2) atoms to form corner-sharing NiO5 square pyramids. The Ni(1)-O(3) bond length is 1.98 Å. Both Ni(1)-O(1) bond lengths are 2.04 Å. Both Ni(1)-O(2) bond lengths are 2.04 Å. There are six inequivalent C sites. In the first 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 1.53 Å. The C(1)-C(3) bond length is 1.39 Å. The C(1)-C(4) bond length is 1.40 Å. In the second C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(1), and one O(2) atom. The C(2)-O(1) bond length is 1.24 Å. The C(2)-O(2) bond length is 1.25 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(1), one C(4), and one C(6) atom. The C(3)-C(4) bond length is 1.43 Å. The C(3)-C(6) bond length is 1.43 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(5) atom. The C(4)-C(5) bond length is 1.44 Å. In the fifth C site, C(5) is bonded in a single-bond geometry to one C(4) and one H(1) atom. The C(5)-H(1) bond length is 0.95 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(3) and one H(2) atom. The C(6)-H(2) bond length is 0.95 Å. There are two 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(2) is bonded in a single-bond geometry to one C(6) atom. There are three inequivalent O sites. In the first O site, O(3) is bonded in a trigonal planar geometry to three equivalent Ni(1) atoms. In the second O site, O(1) is bonded in a distorted single-bond geometry to one Ni(1) and one C(2) atom. In the third O site, O(2) is bonded in a distorted single-bond geometry to one Ni(1) and one C(2) atom. Linkers: 6 [O]C(=O)c1c2ccccc2c(C([O])=O)c2ccccc12. 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: acs. The MOF has largest included sphere 10.78 A, density 0.95 g/cm3, surface area 4116.96 m2/g, accessible volume 0.57 cm3/g