NiCu2C24H28(N3O5)2(CH)4(CH2)2 crystallizes in the trigonal P3_221 space group. The structure consists of twenty-four 02329_fluka molecules and twelve 02329_fluka molecules inside a NiCu2C24H28(N3O5)2 framework. In the NiCu2C24H28(N3O5)2 framework, Ni(1) is bonded in an octahedral geometry to one N(3), one N(4), one N(5), one N(6), one O(10), and one O(5) atom. The Ni(1)-N(3) bond length is 1.96 Å. The Ni(1)-N(4) bond length is 1.99 Å. The Ni(1)-N(5) bond length is 2.09 Å. The Ni(1)-N(6) bond length is 2.13 Å. The Ni(1)-O(10) bond length is 2.12 Å. The Ni(1)-O(5) bond length is 2.12 Å. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a trigonal bipyramidal geometry to one N(1), one O(1), one O(4), one O(7), and one O(8) atom. The Cu(1)-N(1) bond length is 1.91 Å. The Cu(1)-O(1) bond length is 1.99 Å. The Cu(1)-O(4) bond length is 2.00 Å. The Cu(1)-O(7) bond length is 1.92 Å. The Cu(1)-O(8) bond length is 2.33 Å. In the second Cu site, Cu(2) is bonded in a square pyramidal geometry to one N(2), one O(2), one O(3), one O(6), and one O(9) atom. The Cu(2)-N(2) bond length is 1.91 Å. The Cu(2)-O(2) bond length is 2.38 Å. The Cu(2)-O(3) bond length is 1.96 Å. The Cu(2)-O(6) bond length is 2.01 Å. The Cu(2)-O(9) bond length is 1.97 Å. There are twenty-four inequivalent C sites. In the first C site, C(23) is bonded in a distorted trigonal non-coplanar geometry to one N(5), one H(20), and one H(21) atom. The C(23)-N(5) bond length is 1.37 Å. The C(23)-H(20) bond length is 0.99 Å. The C(23)-H(21) bond length is 0.99 Å. In the second C site, C(24) is bonded in a distorted trigonal non-coplanar geometry to one N(3), one H(22), and one H(23) atom. The C(24)-N(3) bond length is 1.31 Å. The C(24)-H(22) bond length is 1.00 Å. The C(24)-H(23) bond length is 0.99 Å. In the third C site, C(25) is bonded in a distorted trigonal non-coplanar geometry to one N(5), one H(24), and one H(25) atom. The C(25)-N(5) bond length is 1.42 Å. The C(25)-H(24) bond length is 1.00 Å. The C(25)-H(25) bond length is 0.98 Å. In the fourth C site, C(26) is bonded in a distorted trigonal non-coplanar geometry to one N(6), one H(26), and one H(27) atom. The C(26)-N(6) bond length is 1.32 Å. The C(26)-H(26) bond length is 0.98 Å. The C(26)-H(27) bond length is 0.99 Å. In the fifth C site, C(28) is bonded in a distorted trigonal non-coplanar geometry to one C(30), one N(4), one H(30), and one H(31) atom. The C(28)-C(30) bond length is 1.51 Å. The C(28)-N(4) bond length is 1.38 Å. The C(28)-H(30) bond length is 0.99 Å. The C(28)-H(31) bond length is 0.99 Å. In the sixth C site, C(29) is bonded in a distorted trigonal non-coplanar geometry to one N(3), one H(33), and one H(34) atom. The C(29)-N(3) bond length is 1.38 Å. The C(29)-H(33) bond length is 0.99 Å. The C(29)-H(34) bond length is 0.99 Å. In the seventh C site, C(30) is bonded in a 4-coordinate geometry to one C(28), one N(6), one H(35), and one H(36) atom. The C(30)-N(6) bond length is 1.53 Å. The C(30)-H(35) bond length is 0.98 Å. The C(30)-H(36) bond length is 0.99 Å. In the eighth C site, C(1) is bonded in a distorted bent 120 degrees geometry to one N(1) and one O(3) atom. The C(1)-N(1) bond length is 1.26 Å. The C(1)-O(3) bond length is 1.31 Å. In the ninth C site, C(2) is bonded in a distorted bent 120 degrees geometry to one O(1) and one O(2) atom. The C(2)-O(1) bond length is 1.33 Å. The C(2)-O(2) bond length is 1.20 Å. In the tenth C site, C(3) is bonded in a distorted bent 120 degrees geometry to one O(4) and one O(5) atom. The C(3)-O(4) bond length is 1.30 Å. The C(3)-O(5) bond length is 1.27 Å. In the eleventh C site, C(4) is bonded in a 2-coordinate geometry to one C(5), one N(1), and one H(1) atom. The C(4)-C(5) bond length is 1.51 Å. The C(4)-N(1) bond length is 1.48 Å. The C(4)-H(1) bond length is 1.00 Å. In the twelfth C site, C(5) is bonded in a trigonal planar geometry to one C(10), one C(4), and one C(6) atom. The C(5)-C(10) bond length is 1.42 Å. The C(5)-C(6) bond length is 1.31 Å. In the thirteenth C site, C(6) is bonded in a distorted single-bond geometry to one C(5), one C(7), and one H(2) atom. The C(6)-C(7) bond length is 1.36 Å. The C(6)-H(2) bond length is 0.96 Å. In the fourteenth C site, C(7) is bonded in a distorted single-bond geometry to one C(6), one C(8), and one H(3) atom. The C(7)-C(8) bond length is 1.37 Å. The C(7)-H(3) bond length is 0.96 Å. In the fifteenth C site, C(8) is bonded in a distorted single-bond geometry to one C(7) and one H(4) atom. The C(8)-H(4) bond length is 0.95 Å. In the sixteenth C site, C(10) is bonded in a single-bond geometry to one C(5) and one H(6) atom. The C(10)-H(6) bond length is 0.95 Å. In the seventeenth C site, C(11) is bonded in a distorted bent 120 degrees geometry to one O(6) and one O(8) atom. The C(11)-O(6) bond length is 1.30 Å. The C(11)-O(8) bond length is 1.21 Å. In the eighteenth C site, C(12) is bonded in a distorted bent 120 degrees geometry to one N(2) and one O(7) atom. The C(12)-N(2) bond length is 1.31 Å. The C(12)-O(7) bond length is 1.26 Å. In the nineteenth C site, C(13) is bonded in a distorted water-like geometry to one C(15), one N(2), and one H(7) atom. The C(13)-C(15) bond length is 1.53 Å. The C(13)-N(2) bond length is 1.45 Å. The C(13)-H(7) bond length is 1.00 Å. In the twentieth C site, C(14) is bonded in a distorted bent 120 degrees geometry to one O(10) and one O(9) atom. The C(14)-O(10) bond length is 1.27 Å. The C(14)-O(9) bond length is 1.27 Å. In the twenty-first C site, C(15) is bonded in a trigonal planar geometry to one C(13), one C(16), and one C(20) atom. The C(15)-C(16) bond length is 1.37 Å. The C(15)-C(20) bond length is 1.39 Å. In the twenty-second C site, C(16) is bonded in a single-bond geometry to one C(15) and one H(8) atom. The C(16)-H(8) bond length is 0.95 Å. In the twenty-third C site, C(20) is bonded in a distorted single-bond geometry to one C(15) and one H(12) atom. The C(20)-H(12) bond length is 0.95 Å. In the twenty-fourth C site, C(22) is bonded in a distorted trigonal non-coplanar geometry to one N(4), one H(18), and one H(19) atom. The C(22)-N(4) bond length is 1.37 Å. The C(22)-H(18) bond length is 0.98 Å. The C(22)-H(19) bond length is 1.00 Å. There are six inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Cu(1), one C(1), and one C(4) atom. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one Cu(2), one C(12), and one C(13) atom. In the third N site, N(3) is bonded in a 4-coordinate geometry to one Ni(1), one C(24), one C(29), and one H(13) atom. The N(3)-H(13) bond length is 1.00 Å. In the fourth N site, N(4) is bonded in a distorted tetrahedral geometry to one Ni(1), one C(22), one C(28), and one H(14) atom. The N(4)-H(14) bond length is 1.00 Å. In the fifth N site, N(5) is bonded in a 4-coordinate geometry to one Ni(1), one C(23), one C(25), and one H(17) atom. The N(5)-H(17) bond length is 1.00 Å. In the sixth N site, N(6) is bonded in a 4-coordinate geometry to one Ni(1), one C(26), one C(30), and one H(32) atom. The N(6)-H(32) bond length is 1.00 Å. There are twenty-eight inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(4) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(6) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(8) atom. In the fifth H site, H(6) is bonded in a single-bond geometry to one C(10) atom. In the sixth H site, H(7) is bonded in a single-bond geometry to one C(13) atom. In the seventh H site, H(8) is bonded in a single-bond geometry to one C(16) atom. In the eighth H site, H(12) is bonded in a single-bond geometry to one C(20) atom. In the ninth H site, H(13) is bonded in a single-bond geometry to one N(3) atom. In the tenth H site, H(14) is bonded in a single-bond geometry to one N(4) atom. In the eleventh H site, H(17) is bonded in a single-bond geometry to one N(5) atom. In the twelfth H site, H(18) is bonded in a single-bond geometry to one C(22) atom. In the thirteenth H site, H(19) is bonded in a single-bond geometry to one C(22) atom. In the fourteenth H site, H(20) is bonded in a single-bond geometry to one C(23) atom. In the fifteenth H site, H(21) is bonded in a single-bond geometry to one C(23) atom. In the sixteenth H site, H(22) is bonded in a single-bond geometry to one C(24) atom. In the seventeenth H site, H(23) is bonded in a single-bond geometry to one C(24) atom. In the eighteenth H site, H(24) is bonded in a single-bond geometry to one C(25) atom. In the nineteenth H site, H(25) is bonded in a single-bond geometry to one C(25) atom. In the twentieth H site, H(26) is bonded in a single-bond geometry to one C(26) atom. In the twenty-first H site, H(27) is bonded in a single-bond geometry to one C(26) atom. In the twenty-second H site, H(30) is bonded in a single-bond geometry to one C(28) atom. In the twenty-third H site, H(31) is bonded in a single-bond geometry to one C(28) atom. In the twenty-fourth H site, H(32) is bonded in a single-bond geometry to one N(6) atom. In the twenty-fifth H site, H(33) is bonded in a single-bond geometry to one C(29) atom. In the twenty-sixth H site, H(34) is bonded in a single-bond geometry to one C(29) atom. In the twenty-seventh H site, H(35) is bonded in a single-bond geometry to one C(30) atom. In the twenty-eighth H site, H(36) is bonded in a single-bond geometry to one C(30) atom. There are ten inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(2) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Cu(2) and one C(2) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Cu(2) and one C(1) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(3) atom. In the fifth O site, O(5) is bonded in a 2-coordinate geometry to one Ni(1) and one C(3) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Cu(2) and one C(11) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(12) atom. In the eighth O site, O(8) is bonded in a water-like geometry to one Cu(1) and one C(11) atom. In the ninth O site, O(9) is bonded in a distorted single-bond geometry to one Cu(2) and one C(14) atom. In the tenth O site, O(10) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(14) atom. Linkers: 4 C1CNCCNCCCNCCNC1. Metal clusters: 12 [Cu] ,6 [Ni]. The MOF has largest included sphere 9.01 A, density 0.84 g/cm3, surface area 4260.33 m2/g, accessible volume 0.72 cm3/g