Ni3C40H32(NO6)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 N(1), one O(1), one O(2), one O(4), and one O(6) atom to form NiNO4 square pyramids that share  a cornercorner with one Ni(2)O6 octahedra,  a cornercorner with one C(19)H3N tetrahedra, and  a cornercorner with one C(20)H3N tetrahedra. The corner-sharing octahedral tilt angles are 69°. The Ni(1)-N(1) bond length is 2.07 Å. The Ni(1)-O(1) bond length is 2.17 Å. The Ni(1)-O(2) bond length is 2.09 Å. The Ni(1)-O(4) bond length is 2.02 Å. The Ni(1)-O(6) bond length is 2.02 Å. In the second Ni site, Ni(2) is bonded to two equivalent O(2), two equivalent O(3), and two equivalent O(5) atoms to form corner-sharing NiO6 octahedra. Both Ni(2)-O(2) bond lengths are 2.11 Å. Both Ni(2)-O(3) bond lengths are 2.03 Å. Both Ni(2)-O(5) bond lengths are 2.02 Å. There are twenty 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 1.50 Å. The C(1)-O(1) bond length is 1.26 Å. The C(1)-O(2) bond length is 1.28 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one C(5) atom. The C(2)-C(3) bond length is 1.36 Å. The C(2)-C(5) bond length is 1.42 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(2) atom. The C(3)-C(4) bond length is 1.42 Å. The C(3)-H(2) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(4), and one C(6) atom. The C(4)-C(4) bond length is 1.38 Å. The C(4)-C(6) bond length is 1.44 Å. In the fifth C site, C(5) is bonded in a distorted single-bond geometry to one C(2) and one H(3) atom. The C(5)-H(3) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(4) 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 distorted bent 120 degrees geometry to one C(8), one O(3), and one O(4) atom. The C(7)-C(8) bond length is 1.51 Å. The C(7)-O(3) bond length is 1.24 Å. The C(7)-O(4) bond length is 1.27 Å. In the eighth C site, C(8) is bonded in a trigonal planar geometry to one C(17), one C(7), and one C(9) atom. The C(8)-C(17) bond length is 1.36 Å. The C(8)-C(9) bond length is 1.40 Å. In the ninth C site, C(9) is bonded in a distorted single-bond geometry to one C(8) and one H(5) atom. The C(9)-H(5) bond length is 0.93 Å. In the tenth C site, C(10) is bonded in a distorted single-bond geometry to one C(16) and one H(6) atom. The C(10)-C(16) bond length is 1.42 Å. The C(10)-H(6) bond length is 0.93 Å. In the eleventh C site, C(11) is bonded in a single-bond geometry to one C(12), one C(16), and one H(7) atom. The C(11)-C(12) bond length is 1.38 Å. The C(11)-C(16) bond length is 1.42 Å. The C(11)-H(7) bond length is 0.93 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(18) atom. The C(12)-C(13) bond length is 1.39 Å. The C(12)-C(18) bond length is 1.52 Å. In the thirteenth C site, C(13) is bonded in a distorted single-bond geometry to one C(12) and one H(8) atom. The C(13)-H(8) bond length is 0.93 Å. In the fourteenth C site, C(14) is bonded in a distorted single-bond geometry to one C(15) and one H(9) atom. The C(14)-C(15) bond length is 1.42 Å. The C(14)-H(9) bond length is 0.93 Å. In the fifteenth C site, C(15) is bonded in a trigonal planar geometry to one C(14), one C(16), and one C(17) atom. The C(15)-C(16) bond length is 1.41 Å. The C(15)-C(17) bond length is 1.41 Å. In the sixteenth C site, C(16) is bonded in a trigonal planar geometry to one C(10), one C(11), and one C(15) atom. In the seventeenth C site, C(17) is bonded in a single-bond geometry to one C(15), one C(8), and one H(10) atom. The C(17)-H(10) bond length is 0.93 Å. In the eighteenth C site, C(18) is bonded in a distorted bent 120 degrees geometry to one C(12), one O(5), and one O(6) atom. The C(18)-O(5) bond length is 1.24 Å. The C(18)-O(6) bond length is 1.26 Å. In the nineteenth C site, C(19) is bonded to one N(1) and three equivalent H(11,12,13) atoms to form CH3N tetrahedra that share  a cornercorner with one Ni(1)NO4 square pyramid and  a cornercorner with one C(20)H3N tetrahedra. The C(19)-N(1) bond length is 1.48 Å. All C(19)-H(11,12,13) bond lengths are 0.96 Å. In the twentieth C site, C(20) is bonded to one N(1), one H(14), one H(15), and one H(16) atom to form CH3N tetrahedra that share  a cornercorner with one Ni(1)NO4 square pyramid and  a cornercorner with one C(19)H3N tetrahedra. The C(20)-N(1) bond length is 1.48 Å. The C(20)-H(14) bond length is 0.96 Å. The C(20)-H(15) bond length is 0.96 Å. The C(20)-H(16) bond length is 0.96 Å. N(1) is bonded in a distorted single-bond geometry to one Ni(1), one C(19), one C(20), and one H(1) atom. The N(1)-H(1) bond length is 0.93 Å. There are fourteen 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 C(3) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(5) 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(9) 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(11) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(13) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(14) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(17) atom. In the eleventh H site, H(11,12,13) is bonded in a single-bond geometry to one C(19) atom. In the twelfth H site, H(14) is bonded in a single-bond geometry to one C(20) atom. In the thirteenth H site, H(15) is bonded in a single-bond geometry to one C(20) atom. In the fourteenth H site, H(16) is bonded in a single-bond geometry to one C(20) atom. There are six inequivalent O sites. In the first O site, O(1) is bonded in a distorted L-shaped geometry to one Ni(1) and one C(1) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to one Ni(1), one Ni(2), and one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Ni(2) and one C(7) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(7) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Ni(2) and one C(18) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(18) atom. Linkers: 6 [O]C(=O)c1ccc2cc(C([O])=O)ccc2c1. Metal clusters: 6 [Ni]. The MOF has largest included sphere 4.96 A, density 1.33 g/cm3, surface area 4402.61 m2/g, accessible volume 0.32 cm3/g