Ni3H6(C5O4)4(CH3)2 crystallizes in the orthorhombic Pbca space group. The structure consists of eight 02329_fluka molecules inside a Ni3H6(C5O4)4 framework. In the Ni3H6(C5O4)4 framework, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(2), one O(3), one O(4), one O(6), one O(7), and one O(8) atom to form distorted corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles are 69°. The Ni(1)-O(2) bond length is 2.01 Å. The Ni(1)-O(3) bond length is 2.17 Å. The Ni(1)-O(4) bond length is 2.06 Å. The Ni(1)-O(6) bond length is 2.02 Å. The Ni(1)-O(7) bond length is 2.19 Å. The Ni(1)-O(8) bond length is 2.04 Å. In the second Ni site, Ni(2) is bonded to two equivalent O(1), two equivalent O(5), and two equivalent O(8) atoms to form corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles are 69°. Both Ni(2)-O(1) bond lengths are 2.05 Å. Both Ni(2)-O(5) bond lengths are 2.02 Å. Both Ni(2)-O(8) bond lengths are 2.09 Å. There are ten inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(6), and one C(7) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-C(6) bond length is 1.39 Å. The C(1)-C(7) bond length is 1.51 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(1), one C(3), and one H(1) atom. The C(2)-C(3) bond length is 1.39 Å. The C(2)-H(1) bond length is 0.95 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(8) atom. The C(3)-C(4) bond length is 1.39 Å. The C(3)-C(8) bond length is 1.49 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one H(2) atom. The C(4)-C(5) bond length is 1.40 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(9) atom. The C(5)-C(6) bond length is 1.39 Å. The C(5)-C(9) bond length is 1.51 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(1), one C(5), and one H(3) atom. The C(6)-H(3) bond length is 0.95 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(1), one O(1), and one O(2) atom. The C(7)-O(1) bond length is 1.26 Å. The C(7)-O(2) bond length is 1.26 Å. In the eighth C site, C(8) is bonded in a bent 120 degrees geometry to one C(3), one O(3), and one O(4) atom. The C(8)-O(3) bond length is 1.26 Å. The C(8)-O(4) bond length is 1.27 Å. In the ninth C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(5), and one O(6) atom. The C(9)-O(5) bond length is 1.24 Å. The C(9)-O(6) bond length is 1.27 Å. In the tenth C site, C(11) is bonded in a distorted bent 120 degrees geometry to one O(7) and one O(8) atom. The C(11)-O(7) bond length is 1.24 Å. The C(11)-O(8) bond length is 1.28 Å. There are three 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. In the third H site, H(3) is bonded in a single-bond geometry to one C(6) atom. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(7) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(7) atom. In the third O site, O(3) is bonded in an L-shaped geometry to one Ni(1) and one C(8) atom. In the fourth O site, O(4) is bonded in an L-shaped geometry to one Ni(1) and one C(8) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Ni(2) and one C(9) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(9) atom. In the seventh O site, O(7) is bonded in a distorted L-shaped geometry to one Ni(1) and one C(11) atom. In the eighth O site, O(8) is bonded in a distorted T-shaped geometry to one Ni(1), one Ni(2), and one C(11) atom. Linkers: 8 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 4 C[C]1O[Ni]23(O[C]O[Ni]4(O[C]O2)O[C]O[Ni]25(O[C]O4)(O[C]O2)O[C](C)O5)(O[C]O3)O1. RCSR code: pyr. The MOF has largest included sphere 5.12 A, density 1.27 g/cm3, surface area 3726.44 m2/g, accessible volume 0.30 cm3/g