Ni3H8(C10O9)2 crystallizes in the monoclinic C2/m space group. 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 64°. The Ni(1)-O(5) bond length is 2.08 Å. Both Ni(1)-O(1) bond lengths are 2.03 Å. Both Ni(1)-O(3) bond lengths are 2.07 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 2.10 Å. All Ni(2)-O(2) bond lengths are 2.04 Å. There are five inequivalent C sites. In the first C site, C(1) is bonded in a single-bond geometry to one C(2), one C(3), and one H(2) atom. The C(1)-C(2) bond length is 1.39 Å. The C(1)-C(3) bond length is 1.40 Å. The C(1)-H(2) bond length is 0.93 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(4) atom. The C(2)-C(3) bond length is 1.40 Å. The C(2)-C(4) bond length is 1.51 Å. In the third C site, C(3) is bonded in a trigonal planar geometry to one C(1), one C(2), and one C(5) atom. The C(3)-C(5) bond length is 1.51 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(4)-O(1) bond length is 1.24 Å. The C(4)-O(2) bond length is 1.26 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(3), one O(3), and one O(4) atom. The C(5)-O(3) bond length is 1.25 Å. The C(5)-O(4) bond length is 1.26 Å. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(5) atom. The H(1)-O(5) bond length is 0.83 Å. In the second H site, H(2) is bonded in a single-bond geometry to one C(1) atom. There are five inequivalent O sites. In the first O site, O(3) is bonded in a distorted single-bond geometry to one Ni(1) and one C(5) atom. In the second O site, O(4) is bonded in a single-bond geometry to one C(5) atom. In the third O site, O(5) is bonded in a distorted water-like geometry to one Ni(1), one Ni(2), and two equivalent H(1) atoms. In the fourth O site, O(1) is bonded in a 2-coordinate geometry to one Ni(1) and one C(4) atom. In the fifth O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(4) atom. Linkers: 4 [O]C(=O)c1cc(C([O])=O)c(C([O])=O)cc1C([O])=O. Metal clusters: 2 O.O.O=[C]O[Ni]1(O[C]=O)O[C]O[Ni]2(O[C]O1)O[C]O[Ni](O[C]=O)(O[C]=O)O[C]O2. RCSR code: scu. The MOF has largest included sphere 5.80 A, density 1.48 g/cm3, surface area 3146.89 m2/g, accessible volume 0.32 cm3/g