NiH3(C3O2)3 crystallizes in the orthorhombic C222_1 space group. Ni(1) is bonded in a 6-coordinate geometry to one O(2), one O(3), one O(4), one O(5), and two equivalent O(6) atoms. The Ni(1)-O(2) bond length is 2.36 Å. The Ni(1)-O(3) bond length is 2.11 Å. The Ni(1)-O(4) bond length is 1.98 Å. The Ni(1)-O(5) bond length is 1.93 Å. There is one shorter (2.11 Å) and one longer (2.30 Å) Ni(1)-O(6) bond length. There are twelve inequivalent C sites. In the first C site, C(1) is bonded in a single-bond geometry to one C(3), one C(8), and one H(1) atom. The C(1)-C(3) bond length is 1.37 Å. The C(1)-C(8) bond length is 1.38 Å. The C(1)-H(1) bond length is 0.93 Å. In the second C site, C(2) is bonded in a bent 120 degrees geometry to one C(3), one O(2), and one O(6) atom. The C(2)-C(3) bond length is 1.54 Å. The C(2)-O(2) bond length is 1.21 Å. The C(2)-O(6) bond length is 1.21 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(9) atom. The C(3)-C(9) bond length is 1.41 Å. In the fourth C site, C(4) is bonded in a bent 120 degrees geometry to one C(6), one O(3), and one O(4) atom. The C(4)-C(6) bond length is 1.50 Å. The C(4)-O(3) bond length is 1.25 Å. The C(4)-O(4) bond length is 1.27 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(12), one C(6), and one H(2) atom. The C(5)-C(12) bond length is 1.40 Å. The C(5)-C(6) bond length is 1.40 Å. The C(5)-H(2) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(10), one C(4), and one C(5) atom. The C(6)-C(10) bond length is 1.38 Å. In the seventh C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(8) and two equivalent O(1) atoms. The C(7)-C(8) bond length is 1.50 Å. Both C(7)-O(1) bond lengths are 1.23 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(7) and two equivalent C(1) atoms. In the ninth C site, C(9) is bonded in a distorted single-bond geometry to two equivalent C(3) and one H(3) atom. The C(9)-H(3) bond length is 0.93 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to two equivalent C(6) and one H(4) atom. The C(10)-H(4) bond length is 0.93 Å. In the eleventh C site, C(11) is bonded in a distorted bent 120 degrees geometry to one C(12) and two equivalent O(5) atoms. The C(11)-C(12) bond length is 1.50 Å. Both C(11)-O(5) bond lengths are 1.26 Å. In the twelfth C site, C(12) is bonded in a trigonal planar geometry to one C(11) and two equivalent C(5) atoms. There are four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(5) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(9) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(10) atom. There are six inequivalent O sites. In the first O site, O(1) is bonded in a single-bond geometry to one C(7) atom. In the second O site, O(2) is bonded in a distorted L-shaped geometry to one Ni(1) and one C(2) atom. In the third O site, O(3) is bonded in an L-shaped geometry to one Ni(1) and one C(4) atom. In the fourth O site, O(4) is bonded in an L-shaped geometry to one Ni(1) and one C(4) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(11) atom. In the sixth O site, O(6) is bonded in a distorted T-shaped geometry to two equivalent Ni(1) and one C(2) atom. Linkers: 3 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1 ,1 [O]C(=O)c1cc([C]=O)cc(C([O])=O)c1. Metal clusters: 2 O=[C]O[Ni]1(O[C]O[Ni]2(O[C]=O)O[C]O2)O[C]O1. RCSR code: gra. The MOF has largest included sphere 5.98 A, density 0.93 g/cm3, surface area 4035.26 m2/g, accessible volume 0.75 cm3/g