Ni5C12H16(N2O9)2(CH2)2(CH)2 crystallizes in the tetragonal P4_32_12 space group. The structure consists of eight 02329_fluka molecules and eight 02329_fluka molecules inside a Ni5C12H16(N2O9)2 framework. In the Ni5C12H16(N2O9)2 framework, there are three inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(1), one O(3), one O(4), one O(6), and two equivalent O(9) atoms to form NiO6 octahedra that share corners with two equivalent Ni(1)O6 octahedra and edges with two equivalent Ni(2)NO5 octahedra. The corner-sharing octahedral tilt angles are 60°. The Ni(1)-O(1) bond length is 2.09 Å. The Ni(1)-O(3) bond length is 2.03 Å. The Ni(1)-O(4) bond length is 2.11 Å. The Ni(1)-O(6) bond length is 2.02 Å. There is one shorter (2.01 Å) and one longer (2.02 Å) Ni(1)-O(9) bond length. In the second Ni site, Ni(2) is bonded to one N(1), one O(1), one O(2), one O(4), one O(5), and one O(9) atom to form NiNO5 octahedra that share  a cornercorner with one Ni(3)N2O4 octahedra and edges with two equivalent Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles are 53°. The Ni(2)-N(1) bond length is 2.06 Å. The Ni(2)-O(1) bond length is 2.05 Å. The Ni(2)-O(2) bond length is 2.00 Å. The Ni(2)-O(4) bond length is 2.11 Å. The Ni(2)-O(5) bond length is 2.12 Å. The Ni(2)-O(9) bond length is 2.01 Å. In the third Ni site, Ni(3) is bonded to two equivalent N(2), two equivalent O(5), and two equivalent O(7) atoms to form corner-sharing NiN2O4 octahedra. The corner-sharing octahedral tilt angles are 53°. Both Ni(3)-N(2) bond lengths are 2.03 Å. Both Ni(3)-O(5) bond lengths are 2.03 Å. Both Ni(3)-O(7) bond lengths are 2.02 Å. There are six 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 1.48 Å. The C(1)-O(1) bond length is 1.38 Å. The C(1)-O(2) bond length is 1.19 Å. In the second C site, C(2) is bonded in a 2-coordinate geometry to one C(1), one N(1), and one H(5) atom. The C(2)-N(1) bond length is 1.49 Å. The C(2)-H(5) bond length is 0.98 Å. In the third C site, C(4) is bonded in a distorted bent 120 degrees geometry to one O(3) and one O(4) atom. The C(4)-O(3) bond length is 1.29 Å. The C(4)-O(4) bond length is 1.25 Å. In the fourth C site, C(5) is bonded in a distorted trigonal planar geometry to one O(5) and one O(6) atom. The C(5)-O(5) bond length is 1.28 Å. The C(5)-O(6) bond length is 1.25 Å. In the fifth C site, C(7) is bonded in a water-like geometry to one C(8), one H(10), and one H(9) atom. The C(7)-C(8) bond length is 1.39 Å. The C(7)-H(10) bond length is 0.99 Å. The C(7)-H(9) bond length is 0.96 Å. In the sixth C site, C(8) is bonded in a distorted trigonal planar geometry to one C(7), one O(7), and one O(8) atom. The C(8)-O(7) bond length is 1.30 Å. The C(8)-O(8) bond length is 1.33 Å. There are two inequivalent N sites. In the first N site, N(1) is bonded in a distorted water-like geometry to one Ni(2), one C(2), one H(1), and one H(2) atom. The N(1)-H(1) bond length is 0.90 Å. The N(1)-H(2) bond length is 0.90 Å. In the second N site, N(2) is bonded in a distorted water-like geometry to one Ni(3), one H(3), and one H(4) atom. The N(2)-H(3) bond length is 0.90 Å. The N(2)-H(4) bond length is 0.90 Å. There are eight inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one N(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one N(1) atom. In the third H site, H(3) is bonded in a single-bond geometry to one N(2) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one N(2) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(2) atom. In the sixth H site, H(9) is bonded in a single-bond geometry to one C(7) atom. In the seventh H site, H(10) is bonded in a single-bond geometry to one C(7) atom. In the eighth H site, H(11) is bonded in a single-bond geometry to one O(9) atom. The H(11)-O(9) bond length is 0.98 Å. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a distorted trigonal non-coplanar geometry to one Ni(1), one Ni(2), and one C(1) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(1) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(4) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Ni(1), one Ni(2), and one C(4) atom. In the fifth O site, O(5) is bonded in a trigonal planar geometry to one Ni(2), one Ni(3), and one C(5) atom. In the sixth O site, O(6) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(5) atom. In the seventh O site, O(7) is bonded in a distorted bent 120 degrees geometry to one Ni(3) and one C(8) atom. In the eighth O site, O(8) is bonded in a single-bond geometry to one C(8) 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(11) atom. Linkers: 16 N[C@H](CC([O])=O)C([O])=O. Metal clusters: 20 [Ni]. The MOF has largest included sphere 6.52 A, density 1.46 g/cm3, surface area 3018.56 m2/g, accessible volume 0.34 cm3/g