NiH6(C5O3)2CH3CH crystallizes in the trigonal P3_121 space group. The structure consists of twelve 02329_fluka molecules and twelve 02329_fluka molecules inside a NiH6(C5O3)2 framework. In the NiH6(C5O3)2 framework, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a rectangular see-saw-like geometry to one O(12), one O(2), one O(6), and one O(9) atom. The Ni(1)-O(12) bond length is 2.13 Å. The Ni(1)-O(2) bond length is 2.04 Å. The Ni(1)-O(6) bond length is 2.04 Å. The Ni(1)-O(9) bond length is 2.10 Å. In the second Ni site, Ni(2) is bonded in a distorted T-shaped geometry to one O(12), one O(3), and one O(9) atom. The Ni(2)-O(12) bond length is 2.09 Å. The Ni(2)-O(3) bond length is 2.04 Å. The Ni(2)-O(9) bond length is 2.06 Å. There are twenty inequivalent C sites. In the first C site, C(2) is bonded in a single-bond geometry to one C(19), one C(3), and one H(4) atom. The C(2)-C(19) bond length is 1.54 Å. The C(2)-C(3) bond length is 1.52 Å. The C(2)-H(4) bond length is 0.98 Å. In the second 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 1.43 Å. The C(3)-C(8) bond length is 1.37 Å. In the third C site, C(4) is bonded in a distorted single-bond geometry to one C(3) and one O(1) atom. The C(4)-O(1) bond length is 1.39 Å. In the fourth C site, C(6) is bonded in a distorted single-bond geometry to one C(7) and one O(4) atom. The C(6)-C(7) bond length is 1.40 Å. The C(6)-O(4) bond length is 1.37 Å. In the fifth C site, C(7) is bonded in a trigonal planar geometry to one C(13), one C(6), and one C(8) atom. The C(7)-C(13) bond length is 1.52 Å. The C(7)-C(8) bond length is 1.39 Å. In the sixth C site, C(8) is bonded in a distorted single-bond geometry to one C(3), one C(7), and one H(6) atom. The C(8)-H(6) bond length is 0.93 Å. In the seventh C site, C(9) is bonded in a distorted trigonal non-coplanar geometry to one C(10); two equivalent H(7,8); and one O(1) atom. The C(9)-C(10) bond length is 1.51 Å. Both C(9)-H(7,8) bond lengths are 0.97 Å. The C(9)-O(1) bond length is 1.42 Å. In the eighth C site, C(10) is bonded in a distorted trigonal planar geometry to one C(9), one O(2), and one O(3) atom. The C(10)-O(2) bond length is 1.25 Å. The C(10)-O(3) bond length is 1.27 Å. In the ninth C site, C(11) is bonded in a distorted trigonal non-coplanar geometry to two equivalent H(9,10) and one O(4) atom. Both C(11)-H(9,10) bond lengths are 0.97 Å. The C(11)-O(4) bond length is 1.43 Å. In the tenth C site, C(12) is bonded in a distorted bent 120 degrees geometry to one O(5) and one O(6) atom. The C(12)-O(5) bond length is 1.25 Å. The C(12)-O(6) bond length is 1.27 Å. In the eleventh C site, C(13) is bonded in a single-bond geometry to one C(15), one C(7), and one H(11) atom. The C(13)-C(15) bond length is 1.53 Å. The C(13)-H(11) bond length is 0.98 Å. In the twelfth C site, C(15) is bonded in a trigonal planar geometry to one C(13), one C(16), and one C(20) atom. The C(15)-C(16) bond length is 1.36 Å. The C(15)-C(20) bond length is 1.40 Å. In the thirteenth C site, C(16) is bonded in a distorted single-bond geometry to one C(15) and one O(7) atom. The C(16)-O(7) bond length is 1.41 Å. In the fourteenth C site, C(18) is bonded in a distorted single-bond geometry to one C(19) and one O(10) atom. The C(18)-C(19) bond length is 1.43 Å. The C(18)-O(10) bond length is 1.36 Å. In the fifteenth C site, C(19) is bonded in a trigonal planar geometry to one C(18), one C(2), and one C(20) atom. The C(19)-C(20) bond length is 1.37 Å. In the sixteenth C site, C(20) is bonded in a distorted single-bond geometry to one C(15), one C(19), and one H(16) atom. The C(20)-H(16) bond length is 0.93 Å. In the seventeenth C site, C(21) is bonded in a distorted trigonal non-coplanar geometry to one C(22); two equivalent H(17,18); and one O(7) atom. The C(21)-C(22) bond length is 1.54 Å. Both C(21)-H(17,18) bond lengths are 0.97 Å. The C(21)-O(7) bond length is 1.39 Å. In the eighteenth C site, C(22) is bonded in a distorted trigonal planar geometry to one C(21), one O(8), and one O(9) atom. The C(22)-O(8) bond length is 1.20 Å. The C(22)-O(9) bond length is 1.28 Å. In the nineteenth C site, C(23) is bonded in a distorted trigonal non-coplanar geometry to one C(24); two equivalent H(19,20); and one O(10) atom. The C(23)-C(24) bond length is 1.50 Å. Both C(23)-H(19,20) bond lengths are 0.97 Å. The C(23)-O(10) bond length is 1.41 Å. In the twentieth C site, C(24) is bonded in a distorted trigonal planar geometry to one C(23), one O(11), and one O(12) atom. The C(24)-O(11) bond length is 1.23 Å. The C(24)-O(12) bond length is 1.25 Å. There are eight inequivalent H sites. In the first H site, H(4) is bonded in a single-bond geometry to one C(2) atom. In the second H site, H(6) is bonded in a single-bond geometry to one C(8) atom. In the third H site, H(7,8) is bonded in a single-bond geometry to one C(9) atom. In the fourth H site, H(9,10) is bonded in a single-bond geometry to one C(11) atom. In the fifth H site, H(11) is bonded in a single-bond geometry to one C(13) atom. In the sixth H site, H(16) is bonded in a single-bond geometry to one C(20) atom. In the seventh H site, H(17,18) is bonded in a single-bond geometry to one C(21) atom. In the eighth H site, H(19,20) is bonded in a single-bond geometry to one C(23) atom. There are twelve inequivalent O sites. In the first O site, O(5) is bonded in a single-bond geometry to one C(12) atom. In the second O site, O(6) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(12) atom. In the third O site, O(7) is bonded in a water-like geometry to one C(16) and one C(21) atom. In the fourth O site, O(8) is bonded in a single-bond geometry to one C(22) atom. In the fifth O site, O(9) is bonded in a distorted trigonal planar geometry to one Ni(1), one Ni(2), and one C(22) atom. In the sixth O site, O(10) is bonded in a bent 120 degrees geometry to one C(18) and one C(23) atom. In the seventh O site, O(11) is bonded in a single-bond geometry to one C(24) atom. In the eighth O site, O(12) is bonded in a 3-coordinate geometry to one Ni(1), one Ni(2), and one C(24) atom. In the ninth O site, O(1) is bonded in a bent 120 degrees geometry to one C(4) and one C(9) atom. In the tenth O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(10) atom. In the eleventh O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(10) atom. In the twelfth O site, O(4) is bonded in a bent 120 degrees geometry to one C(11) and one C(6) atom. Linkers: 3 C[C@H]1c2cc(c(OCC([O])=O)cc2OCC([O])=O)[C@@H](C)c2cc(c(OCC([O])=O)cc2OCC([O])=O)[C@@H](C)c2cc(c(OCC([O])=O)cc2OCC([O])=O)[C@@H](C)c2cc1c(OCC([O])=O)cc2OCC([O])=O. Metal clusters: 6 O=[C]O[Ni]O[C]O[Ni](O[C]=O)O[C]=O. RCSR code: anh. The MOF has largest included sphere 7.05 A, density 1.03 g/cm3, surface area 4316.45 m2/g, accessible volume 0.54 cm3/g