Ni3H12(C18O13)2 crystallizes in the monoclinic P2_1/c space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(1), one O(10), one O(12), one O(13), one O(4), and one O(7) atom to form corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles are 68°. The Ni(1)-O(1) bond length is 2.03 Å. The Ni(1)-O(10) bond length is 2.01 Å. The Ni(1)-O(12) bond length is 2.06 Å. The Ni(1)-O(13) bond length is 2.07 Å. The Ni(1)-O(4) bond length is 1.99 Å. The Ni(1)-O(7) bond length is 2.13 Å. In the second Ni site, Ni(2) is bonded to two equivalent O(13), two equivalent O(3), and two equivalent O(9) atoms to form corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles are 68°. Both Ni(2)-O(13) bond lengths are 2.11 Å. Both Ni(2)-O(3) bond lengths are 2.07 Å. Both Ni(2)-O(9) bond lengths are 2.02 Å. There are eighteen 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 1.50 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 1.39 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 1.49 Å. In the sixth C site, C(6) is bonded in a 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 1.28 Å. The C(7)-O(2) bond length is 1.24 Å. In the eighth C site, C(8) is bonded in a distorted 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 1.26 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 1.34 Å. The C(9)-O(6) bond length is 1.20 Å. In the tenth C site, C(10) is bonded in a trigonal planar geometry to one C(11), one C(15), and one C(16) atom. The C(10)-C(11) bond length is 1.39 Å. The C(10)-C(15) bond length is 1.39 Å. The C(10)-C(16) bond length is 1.50 Å. In the eleventh C site, C(11) is bonded in a distorted single-bond geometry to one C(10), one C(12), and one H(4) atom. The C(11)-C(12) bond length is 1.38 Å. The C(11)-H(4) bond length is 0.95 Å. In the twelfth C site, C(12) is bonded in a trigonal planar geometry to one C(11), one C(13), and one C(17) atom. The C(12)-C(13) bond length is 1.39 Å. The C(12)-C(17) bond length is 1.53 Å. In the thirteenth C site, C(13) is bonded in a distorted single-bond geometry to one C(12), one C(14), and one H(5) atom. The C(13)-C(14) bond length is 1.39 Å. The C(13)-H(5) bond length is 0.95 Å. In the fourteenth C site, C(14) is bonded in a trigonal planar geometry to one C(13), one C(15), and one C(18) atom. The C(14)-C(15) bond length is 1.39 Å. The C(14)-C(18) bond length is 1.51 Å. In the fifteenth C site, C(15) is bonded in a single-bond geometry to one C(10), one C(14), and one H(6) atom. The C(15)-H(6) bond length is 0.95 Å. In the sixteenth C site, C(16) is bonded in a bent 120 degrees geometry to one C(10), one O(7), and one O(8) atom. The C(16)-O(7) bond length is 1.23 Å. The C(16)-O(8) bond length is 1.33 Å. In the seventeenth C site, C(17) is bonded in a distorted bent 120 degrees geometry to one C(12), one O(10), and one O(9) atom. The C(17)-O(10) bond length is 1.26 Å. The C(17)-O(9) bond length is 1.25 Å. In the eighteenth C site, C(18) is bonded in a distorted bent 120 degrees geometry to one C(14), one O(11), and one O(12) atom. The C(18)-O(11) bond length is 1.24 Å. The C(18)-O(12) bond length is 1.28 Å. There are six 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. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(11) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(13) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(15) atom. There are thirteen inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(7) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(7) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(8) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(8) atom. In the fifth O site, O(5) is bonded in a single-bond geometry to one C(9) atom. In the sixth O site, O(6) is bonded in a single-bond geometry to one C(9) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(16) atom. In the eighth O site, O(8) is bonded in a single-bond geometry to one C(16) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(17) atom. In the tenth O site, O(10) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(17) atom. In the eleventh O site, O(11) is bonded in a single-bond geometry to one C(18) atom. In the twelfth O site, O(12) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(18) atom. In the thirteenth O site, O(13) is bonded in a water-like geometry to one Ni(1) and one Ni(2) atom. Linkers: 8 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 2 [O][C]O[Ni]12(O[C]=O)(O[C]=O)O[C]O[Ni]34(O[C]O1)(O[C]O[Ni](O[C][O])(O[C]=O)(O[C]=O)(O[C]O3)O4)O2. RCSR code: tfz-d. The MOF has largest included sphere 5.89 A, density 1.24 g/cm3, surface area 3769.39 m2/g, accessible volume 0.41 cm3/g