Ni3H16(C9O7)2 crystallizes in the triclinic P-1 space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(3), one O(4), one O(7), and two equivalent O(2) atoms to form NiO5 square pyramids that share  a cornercorner with one Ni(2)O6 octahedra and  an edgeedge with one Ni(1)O5 square pyramid. The corner-sharing octahedral tilt angles are 69°. The Ni(1)-O(3) bond length is 2.08 Å. The Ni(1)-O(4) bond length is 2.00 Å. The Ni(1)-O(7) bond length is 2.01 Å. Both Ni(1)-O(2) bond lengths are 2.05 Å. In the second Ni site, Ni(2) is bonded to two equivalent O(1), two equivalent O(3), and two equivalent O(5) atoms to form corner-sharing NiO6 octahedra. Both Ni(2)-O(1) bond lengths are 2.07 Å. Both Ni(2)-O(3) bond lengths are 2.14 Å. Both Ni(2)-O(5) bond lengths are 2.03 Å. There are nine 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 1.53 Å. The C(1)-O(1) bond length is 1.24 Å. The C(1)-O(2) bond length is 1.29 Å. In the second C site, C(2) is bonded in a trigonal non-coplanar geometry to one C(1), one C(3), and one C(7) atom. The C(2)-C(3) bond length is 1.54 Å. The C(2)-C(7) 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), one H(1), and one H(2) atom. The C(3)-C(4) bond length is 1.52 Å. The C(3)-H(1) bond length is 0.95 Å. The C(3)-H(2) bond length is 0.95 Å. In the fourth C site, C(4) is bonded in a trigonal non-coplanar geometry to one C(3), one C(5), and one C(8) atom. The C(4)-C(5) bond length is 1.54 Å. The C(4)-C(8) bond length is 1.52 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 1.54 Å. Both C(5)-H(3,4) bond lengths are 0.95 Å. In the sixth C site, C(6) is bonded in a trigonal non-coplanar geometry to one C(5), one C(7), and one C(9) atom. The C(6)-C(7) bond length is 1.54 Å. The C(6)-C(9) bond length is 1.54 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 distorted bent 120 degrees geometry to one C(4), one O(6), and one O(7) atom. The C(8)-O(6) bond length is 1.24 Å. The C(8)-O(7) 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(6), one O(4), and one O(5) atom. The C(9)-O(4) bond length is 1.24 Å. The C(9)-O(5) 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(3) atom. 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(3,4) is bonded in a single-bond geometry to one C(5) atom. In the fourth H site, H(5,6) is bonded in a single-bond geometry to one C(7) atom. In the fifth H site, H(7) is bonded in a single-bond geometry to one O(3) atom. The H(7)-O(3) bond length is 0.95 Å. In the sixth H site, H(8) is bonded in a single-bond geometry to one O(3) atom. The H(8)-O(3) bond length is 0.95 Å. There are seven inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(1) atom. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to two equivalent Ni(1) and one C(1) atom. In the third O site, O(3) is bonded in a distorted water-like geometry to one Ni(1), one Ni(2), one H(7), and one H(8) atom. In the fourth O site, O(4) is bonded in a distorted bent 150 degrees geometry to one Ni(1) and one C(9) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(9) atom. In the sixth O site, O(6) is bonded in a single-bond geometry to one C(8) atom. In the seventh O site, O(7) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(8) atom. Linkers: 2 [O]C(=O)[C]1C[C](C([O])=O)C[C](C([O])=O)C1. Metal clusters: 3 [Ni]. The MOF has largest included sphere 3.91 A, density 1.57 g/cm3, surface area 3295.43 m2/g, accessible volume 0.24 cm3/g