NiH8(CO4)2(CH2)4 crystallizes in the monoclinic P2_1/c space group. The structure consists of eight 02329_fluka molecules inside a NiH8(CO4)2 framework. In the NiH8(CO4)2 framework, Ni(1) is bonded in an octahedral geometry to two equivalent O(1), two equivalent O(2), and two equivalent O(3) atoms. Both Ni(1)-O(1) bond lengths are 2.07 Å. Both Ni(1)-O(2) bond lengths are 2.10 Å. Both Ni(1)-O(3) bond lengths are 2.08 Å. C(1) is bonded in a distorted bent 120 degrees geometry to one O(3) and one O(4) atom. The C(1)-O(3) bond length is 1.29 Å. The C(1)-O(4) bond length is 1.27 Å. There are four inequivalent H sites. In the first H site, H(1) is bonded in a distorted single-bond geometry to one O(1) and one O(4) atom. The H(1)-O(1) bond length is 1.01 Å. The H(1)-O(4) bond length is 1.66 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(1) atom. The H(2)-O(1) bond length is 0.99 Å. In the third H site, H(3) is bonded in a distorted single-bond geometry to one O(2) and one O(3) atom. The H(3)-O(2) bond length is 1.01 Å. The H(3)-O(3) bond length is 1.64 Å. In the fourth H site, H(4) is bonded in a single-bond geometry to one O(2) and one O(4) atom. The H(4)-O(2) bond length is 1.00 Å. The H(4)-O(4) bond length is 1.71 Å. There are four inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1), one H(1), and one H(2) atom. In the second O site, O(2) is bonded in a distorted water-like geometry to one Ni(1), one H(3), and one H(4) atom. In the third O site, O(3) is bonded in a distorted trigonal planar geometry to one Ni(1), one C(1), and one H(3) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one C(1), one H(1), and one H(4) atom. Linkers: 2 [O]C(=O)CCCCC([O])=O. Metal clusters: 2 O.O.O.O.O=[C]O[Ni]O[C]=O. The MOF has largest included sphere 1.95 A, density 1.75 g/cm3, surface area 3941.17 m2/g, accessible volume 0.14 cm3/g