Ni2C16H7O9 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(3), one O(8), and two equivalent O(9) atoms to form NiO5 square pyramids that share corners with two equivalent Ni(2)O6 octahedra and  an edgeedge with one Ni(1)O5 square pyramid. The corner-sharing octahedral tilt angles range from 55-70°. The Ni(1)-O(1) bond length is 2.10 Å. The Ni(1)-O(3) bond length is 2.06 Å. The Ni(1)-O(8) bond length is 2.05 Å. There is one shorter (2.01 Å) and one longer (2.04 Å) Ni(1)-O(9) bond length. In the second Ni site, Ni(2) is bonded to one O(2), one O(4), one O(5), one O(6), one O(7), and one O(9) atom to form corner-sharing NiO6 octahedra. The Ni(2)-O(2) bond length is 2.02 Å. The Ni(2)-O(4) bond length is 2.09 Å. The Ni(2)-O(5) bond length is 2.19 Å. The Ni(2)-O(6) bond length is 2.11 Å. The Ni(2)-O(7) bond length is 2.05 Å. The Ni(2)-O(9) bond length is 1.98 Å. There are sixteen 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 1.41 Å. The C(1)-C(6) bond length is 1.40 Å. The C(1)-C(7) bond length is 1.48 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(13), and one C(3) atom. The C(2)-C(13) bond length is 1.51 Å. The C(2)-C(3) bond length is 1.40 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2) and one H(2) atom. The C(3)-H(2) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(5) and one H(3) atom. The C(4)-C(5) bond length is 1.38 Å. The C(4)-H(3) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(14), one C(4), and one C(6) atom. The C(5)-C(14) bond length is 1.50 Å. The C(5)-C(6) bond length is 1.39 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(1), one C(5), and one H(4) atom. The C(6)-H(4) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a trigonal planar geometry to one C(1), one C(12), and one C(8) atom. The C(7)-C(12) bond length is 1.40 Å. The C(7)-C(8) bond length is 1.39 Å. In the eighth C site, C(8) is bonded in a distorted single-bond geometry to one C(7), one C(9), and one H(5) atom. The C(8)-C(9) bond length is 1.40 Å. The C(8)-H(5) bond length is 0.93 Å. In the ninth C site, C(9) is bonded in a trigonal planar geometry to one C(10), one C(15), and one C(8) atom. The C(9)-C(10) bond length is 1.39 Å. The C(9)-C(15) bond length is 1.48 Å. In the tenth C site, C(10) is bonded in a distorted trigonal planar geometry to one C(11), one C(9), and one H(6) atom. The C(10)-C(11) bond length is 1.39 Å. The C(10)-H(6) bond length is 0.93 Å. In the eleventh C site, C(11) is bonded in a trigonal planar geometry to one C(10), one C(12), and one C(16) atom. The C(11)-C(12) bond length is 1.39 Å. The C(11)-C(16) bond length is 1.52 Å. In the twelfth C site, C(12) is bonded in a single-bond geometry to one C(11), one C(7), and one H(7) atom. The C(12)-H(7) bond length is 0.93 Å. In the thirteenth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(2), one O(1), and one O(2) atom. The C(13)-O(1) bond length is 1.24 Å. The C(13)-O(2) bond length is 1.27 Å. In the fourteenth C site, C(14) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(3), and one O(4) atom. The C(14)-O(3) bond length is 1.26 Å. The C(14)-O(4) bond length is 1.27 Å. In the fifteenth C site, C(15) is bonded in a bent 120 degrees geometry to one C(9), one O(5), and one O(6) atom. The C(15)-O(5) bond length is 1.26 Å. The C(15)-O(6) bond length is 1.27 Å. In the sixteenth C site, C(16) is bonded in a distorted bent 120 degrees geometry to one C(11), one O(7), and one O(8) atom. The C(16)-O(7) bond length is 1.26 Å. The C(16)-O(8) bond length is 1.25 Å. There are seven inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(9) atom. The H(1)-O(9) bond length is 0.98 Å. In the second H site, H(2) is bonded in a single-bond geometry to one C(3) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(4) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(6) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(8) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(10) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(12) atom. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(13) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(13) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(14) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(14) atom. In the fifth O site, O(5) is bonded in an L-shaped geometry to one Ni(2) and one C(15) atom. In the sixth O site, O(6) is bonded in an L-shaped geometry to one Ni(2) and one C(15) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(16) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(16) atom. In the ninth O site, O(9) is bonded in a distorted single-bond geometry to one Ni(2), two equivalent Ni(1), and one H(1) atom. Linkers: 4 [O]C(=O)c1cc(C([O])=O)cc(-c2cc(C([O])=O)ccc2C([O])=O)c1. Metal clusters: 2 O[Ni]123(O[C]O[Ni](O[C]O1)O[C]O[Ni]14(O)(O[C]O[Ni](O[C]O1)O[C]O2)O[C]O4)O[C]O3. RCSR code: flu. The MOF has largest included sphere 6.23 A, density 1.33 g/cm3, surface area 3401.07 m2/g, accessible volume 0.33 cm3/g