Ni2C14H14O9 crystallizes in the orthorhombic P2_12_12_1 space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a distorted T-shaped geometry to one O(1), one O(4), and one O(9) atom. The Ni(1)-O(1) bond length is 2.04 Å. The Ni(1)-O(4) bond length is 1.99 Å. The Ni(1)-O(9) bond length is 2.10 Å. In the second Ni site, Ni(2) is bonded in an octahedral geometry to one O(2), one O(3), one O(5), one O(6), one O(8), and one O(9) atom. The Ni(2)-O(2) bond length is 2.03 Å. The Ni(2)-O(3) bond length is 1.98 Å. The Ni(2)-O(5) bond length is 2.12 Å. The Ni(2)-O(6) bond length is 2.13 Å. The Ni(2)-O(8) bond length is 2.03 Å. The Ni(2)-O(9) bond length is 2.09 Å. There are fourteen inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(1)-C(2) bond length is 1.55 Å. The C(1)-O(1) bond length is 1.27 Å. The C(1)-O(2) bond length is 1.25 Å. In the second C site, C(2) is bonded to one C(1), one C(3), one C(7), and one C(8) atom to form corner-sharing CC4 tetrahedra. The C(2)-C(3) bond length is 1.53 Å. The C(2)-C(7) bond length is 1.55 Å. The C(2)-C(8) bond length is 1.55 Å. In the third C site, C(3) is bonded in a water-like geometry to one C(2); one C(4); and two equivalent H(1,2) atoms. The C(3)-C(4) bond length is 1.55 Å. Both C(3)-H(1,2) bond lengths are 0.95 Å. In the fourth C site, C(4) is bonded to one C(10), one C(12), one C(3), and one C(5) atom to form corner-sharing CC4 tetrahedra. The C(4)-C(10) bond length is 1.54 Å. The C(4)-C(12) bond length is 1.54 Å. The C(4)-C(5) bond length is 1.54 Å. In the fifth C site, C(5) is bonded in a water-like geometry to one C(4); one C(6); and two equivalent H(3,4) atoms. The C(5)-C(6) bond length is 1.53 Å. Both C(5)-H(3,4) bond lengths are 0.95 Å. In the sixth C site, C(6) is bonded to one C(11), one C(13), one C(5), and one C(7) atom to form corner-sharing CC4 tetrahedra. The C(6)-C(11) bond length is 1.54 Å. The C(6)-C(13) bond length is 1.52 Å. The C(6)-C(7) bond length is 1.55 Å. In the seventh C site, C(7) is bonded in a water-like geometry to one C(2); one C(6); and two equivalent H(5,6) atoms. Both C(7)-H(5,6) bond lengths are 0.95 Å. In the eighth C site, C(8) is bonded in a water-like geometry to one C(2); one C(9); and two equivalent H(7,8) atoms. The C(8)-C(9) bond length is 1.53 Å. Both C(8)-H(7,8) bond lengths are 0.95 Å. In the ninth C site, C(9) is bonded to one C(10), one C(11), one C(14), and one C(8) atom to form corner-sharing CC4 tetrahedra. The C(9)-C(10) bond length is 1.52 Å. The C(9)-C(11) bond length is 1.54 Å. The C(9)-C(14) bond length is 1.54 Å. In the tenth C site, C(10) is bonded in a water-like geometry to one C(4), one C(9), one H(10), and one H(9) atom. The C(10)-H(10) bond length is 0.95 Å. The C(10)-H(9) bond length is 0.95 Å. In the eleventh C site, C(11) is bonded in a water-like geometry to one C(6), one C(9), one H(11), and one H(12) atom. The C(11)-H(11) bond length is 0.95 Å. The C(11)-H(12) bond length is 0.95 Å. In the twelfth C site, C(12) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(12)-O(3) bond length is 1.24 Å. The C(12)-O(4) bond length is 1.27 Å. In the thirteenth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(6), one O(5), and one O(6) atom. The C(13)-O(5) bond length is 1.27 Å. The C(13)-O(6) bond length is 1.26 Å. In the fourteenth C site, C(14) is bonded in a distorted bent 120 degrees geometry to one C(9), one O(7), and one O(8) atom. The C(14)-O(7) bond length is 1.29 Å. The C(14)-O(8) bond length is 1.22 Å. There are ten inequivalent H sites. In the first H site, H(1,2) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(3,4) is bonded in a single-bond geometry to one C(5) atom. In the third H site, H(5,6) is bonded in a single-bond geometry to one C(7) atom. In the fourth H site, H(7,8) is bonded in a single-bond geometry to one C(8) atom. In the fifth H site, H(9) is bonded in a single-bond geometry to one C(10) atom. In the sixth H site, H(10) is bonded in a single-bond geometry to one C(10) atom. In the seventh H site, H(11) is bonded in a single-bond geometry to one C(11) atom. In the eighth H site, H(12) is bonded in a single-bond geometry to one C(11) atom. In the ninth H site, H(13) is bonded in a single-bond geometry to one O(9) atom. The H(13)-O(9) bond length is 0.90 Å. In the tenth H site, H(14) is bonded in a single-bond geometry to one O(9) atom. The H(14)-O(9) bond length is 0.80 Å. There are nine inequivalent O sites. In the first O site, O(9) is bonded in a distorted bent 120 degrees geometry to one Ni(1), one Ni(2), one H(13), and one H(14) atom. In the second O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(1) atom. In the third O site, O(2) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(1) atom. In the fourth O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(12) atom. In the fifth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Ni(1) and one C(12) atom. In the sixth O site, O(5) is bonded in an L-shaped geometry to one Ni(2) and one C(13) atom. In the seventh O site, O(6) is bonded in a distorted L-shaped geometry to one Ni(2) and one C(13) atom. In the eighth O site, O(7) is bonded in a single-bond geometry to one C(14) atom. In the ninth O site, O(8) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(14) atom. Linkers: 4 [O]C(=O)[C@]12C[C@]3(C([O])=O)C[C@](C([O])=O)(C1)C[C@](C([O])=O)(C2)C3. Metal clusters: 4 O.O=[C]O[Ni]12(O[C]O[Ni]O[C]O1)O[C]O2. RCSR code: sra. The MOF has largest included sphere 4.23 A, density 1.37 g/cm3, surface area 3421.04 m2/g, accessible volume 0.35 cm3/g