NiCu4C56H21(NO4)4 crystallizes in the tetragonal P4/mbm space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a rectangular see-saw-like geometry to two equivalent N(3) and two equivalent N(5) atoms. Both Ni(1)-N(3) bond lengths are 1.95 Å. Both Ni(1)-N(5) bond lengths are 1.96 Å. In the second Ni site, Ni(2) is bonded in a square co-planar geometry to one N(1), one N(2), and two equivalent N(4) atoms. The Ni(2)-N(1) bond length is 1.98 Å. The Ni(2)-N(2) bond length is 1.89 Å. Both Ni(2)-N(4) bond lengths are 1.92 Å. There are two inequivalent Cu sites. In the first Cu site, Cu(1) is bonded in a distorted rectangular see-saw-like geometry to one O(1), one O(4), one O(5), and one O(7) atom. The Cu(1)-O(1) bond length is 1.94 Å. The Cu(1)-O(4) bond length is 1.92 Å. The Cu(1)-O(5) bond length is 1.91 Å. The Cu(1)-O(7) bond length is 1.83 Å. In the second Cu site, Cu(2) is bonded in a distorted rectangular see-saw-like geometry to one O(2), one O(3), one O(6), and one O(8) atom. The Cu(2)-O(2) bond length is 1.97 Å. The Cu(2)-O(3) bond length is 1.92 Å. The Cu(2)-O(6) bond length is 1.96 Å. The Cu(2)-O(8) bond length is 1.96 Å. There are thirty-five inequivalent C sites. In the first C site, C(28) is bonded in a distorted trigonal planar geometry to one C(27), one C(29), and one N(4) atom. The C(28)-C(27) bond length is 1.41 Å. The C(28)-C(29) bond length is 1.48 Å. The C(28)-N(4) bond length is 1.28 Å. In the second C site, C(22) is bonded in a distorted single-bond geometry to one C(23) and one H(9) atom. The C(22)-C(23) bond length is 1.45 Å. The C(22)-H(9) bond length is 0.93 Å. In the third C site, C(23) is bonded in a distorted trigonal planar geometry to one C(22), one C(24), and one N(1) atom. The C(23)-C(24) bond length is 1.38 Å. The C(23)-N(1) bond length is 1.36 Å. In the fourth C site, C(24) is bonded in a trigonal planar geometry to one C(23), one C(25), and one C(32) atom. The C(24)-C(25) bond length is 1.36 Å. The C(24)-C(32) bond length is 1.51 Å. In the fifth C site, C(25) is bonded in a distorted trigonal planar geometry to one C(24), one C(26), and one N(4) atom. The C(25)-C(26) bond length is 1.41 Å. The C(25)-N(4) bond length is 1.36 Å. In the sixth C site, C(26) is bonded in a distorted single-bond geometry to one C(25) and one H(10) atom. The C(26)-H(10) bond length is 0.93 Å. In the seventh C site, C(27) is bonded in a distorted single-bond geometry to one C(28) and one H(11) atom. The C(27)-H(11) bond length is 0.93 Å. In the eighth C site, C(34) is bonded in a 3-coordinate geometry to one C(35) and two equivalent C(17) atoms. The C(34)-C(35) bond length is 1.74 Å. Both C(34)-C(17) bond lengths are 1.39 Å. In the ninth C site, C(35) is bonded in a T-shaped geometry to one C(34) and two equivalent C(18) atoms. Both C(35)-C(18) bond lengths are 1.63 Å. In the tenth C site, C(29) is bonded in a distorted tetrahedral geometry to one C(28), one C(30), and two equivalent C(17) atoms. The C(29)-C(30) bond length is 1.47 Å. Both C(29)-C(17) bond lengths are 1.80 Å. In the eleventh C site, C(30) is bonded in a distorted trigonal planar geometry to one C(29), one C(31), and one N(2) atom. The C(30)-C(31) bond length is 1.44 Å. The C(30)-N(2) bond length is 1.27 Å. In the twelfth C site, C(1) is bonded in a distorted single-bond geometry to one C(2) and one H(1) atom. The C(1)-C(2) bond length is 1.45 Å. The C(1)-H(1) bond length is 0.93 Å. In the thirteenth C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(3), and one N(3) atom. The C(2)-C(3) bond length is 1.35 Å. The C(2)-N(3) bond length is 1.38 Å. In the fourteenth C site, C(3) is bonded in a trigonal planar geometry to one C(2), one C(4), and one C(6) atom. The C(3)-C(4) bond length is 1.38 Å. The C(3)-C(6) bond length is 1.56 Å. In the fifteenth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(3), one C(5), and one N(5) atom. The C(4)-C(5) bond length is 1.46 Å. The C(4)-N(5) bond length is 1.36 Å. In the sixteenth C site, C(5) is bonded in a distorted single-bond geometry to one C(4) and one H(2) atom. The C(5)-H(2) bond length is 0.93 Å. In the seventeenth C site, C(6) is bonded in a trigonal planar geometry to one C(11), one C(3), and one C(7) atom. The C(6)-C(11) bond length is 1.35 Å. The C(6)-C(7) bond length is 1.37 Å. In the eighteenth 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 1.39 Å. The C(7)-H(3) bond length is 0.93 Å. In the nineteenth C site, C(8) is bonded in a trigonal planar geometry to one C(12), one C(7), and one C(9) atom. The C(8)-C(12) bond length is 1.47 Å. The C(8)-C(9) bond length is 1.40 Å. In the twentieth C site, C(9) is bonded in a distorted trigonal planar geometry to one C(10), one C(8), and one H(4) atom. The C(9)-C(10) bond length is 1.40 Å. The C(9)-H(4) bond length is 0.93 Å. In the twenty-first C site, C(10) is bonded in a trigonal planar geometry to one C(11), one C(13), and one C(9) atom. The C(10)-C(11) bond length is 1.37 Å. The C(10)-C(13) bond length is 1.53 Å. In the twenty-second C site, C(11) is bonded in a distorted single-bond geometry to one C(10), one C(6), and one H(5) atom. The C(11)-H(5) bond length is 0.93 Å. In the twenty-third C site, C(12) is bonded in a bent 120 degrees geometry to one C(8), one O(1), and one O(2) atom. The C(12)-O(1) bond length is 1.24 Å. The C(12)-O(2) bond length is 1.25 Å. In the twenty-fourth C site, C(13) is bonded in a bent 120 degrees geometry to one C(10), one O(3), and one O(4) atom. The C(13)-O(3) bond length is 1.24 Å. The C(13)-O(4) bond length is 1.31 Å. In the twenty-fifth C site, C(14) is bonded in a distorted single-bond geometry to one C(15), one C(32), and one H(6) atom. The C(14)-C(15) bond length is 1.42 Å. The C(14)-C(32) bond length is 1.44 Å. The C(14)-H(6) bond length is 0.93 Å. In the twenty-sixth C site, C(15) is bonded in a trigonal planar geometry to one C(14), one C(16), and one C(33) atom. The C(15)-C(16) bond length is 1.51 Å. The C(15)-C(33) bond length is 1.40 Å. In the twenty-seventh C site, C(16) is bonded in a distorted bent 120 degrees geometry to one C(15), one O(5), and one O(6) atom. The C(16)-O(5) bond length is 1.27 Å. The C(16)-O(6) bond length is 1.29 Å. In the twenty-eighth C site, C(17) is bonded in a 3-coordinate geometry to one C(20), one C(29), and one C(34) atom. The C(17)-C(20) bond length is 1.34 Å. In the twenty-ninth C site, C(18) is bonded in a distorted single-bond geometry to one C(19), one C(35), and one H(7) atom. The C(18)-C(19) bond length is 1.66 Å. The C(18)-H(7) bond length is 0.93 Å. In the thirtieth C site, C(19) is bonded in a trigonal planar geometry to one C(18), one C(20), and one C(21) atom. The C(19)-C(20) bond length is 1.31 Å. The C(19)-C(21) bond length is 1.42 Å. In the thirty-first C site, C(20) is bonded in a distorted trigonal planar geometry to one C(17), one C(19), and one H(8) atom. The C(20)-H(8) bond length is 0.93 Å. In the thirty-second C site, C(21) is bonded in a distorted bent 120 degrees geometry to one C(19), one O(7), and one O(8) atom. The C(21)-O(7) bond length is 1.22 Å. The C(21)-O(8) bond length is 1.34 Å. In the thirty-third C site, C(31) is bonded in a distorted single-bond geometry to one C(30) and one H(12) atom. The C(31)-H(12) bond length is 0.93 Å. In the thirty-fourth C site, C(32) is bonded in a trigonal planar geometry to one C(24) and two equivalent C(14) atoms. In the thirty-fifth C site, C(33) is bonded in a distorted single-bond geometry to two equivalent C(15) and one H(13) atom. The C(33)-H(13) bond length is 0.93 Å. There are five inequivalent N sites. In the first N site, N(1) is bonded in a distorted trigonal planar geometry to one Ni(2) and two equivalent C(23) atoms. In the second N site, N(2) is bonded in a distorted trigonal planar geometry to one Ni(2) and two equivalent C(30) atoms. In the third N site, N(3) is bonded in a distorted trigonal planar geometry to one Ni(1) and two equivalent C(2) atoms. In the fourth N site, N(4) is bonded in a 3-coordinate geometry to one Ni(2), one C(25), and one C(28) atom. In the fifth N site, N(5) is bonded in a distorted trigonal planar geometry to one Ni(1) and two equivalent C(4) atoms. There are thirteen inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(5) 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(9) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(11) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(14) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(18) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(20) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(22) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(26) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(27) atom. In the twelfth H site, H(12) is bonded in a single-bond geometry to one C(31) atom. In the thirteenth H site, H(13) is bonded in a single-bond geometry to one C(33) atom. There are eight inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Cu(1) and one C(12) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Cu(2) and one C(12) atom. In the third O site, O(3) is bonded in a distorted single-bond geometry to one Cu(2) and one C(13) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Cu(1) and one C(13) atom. In the fifth O site, O(5) is bonded in a distorted single-bond geometry to one Cu(1) and one C(16) atom. In the sixth O site, O(6) is bonded in a distorted bent 120 degrees geometry to one Cu(2) and one C(16) atom. In the seventh O site, O(7) is bonded in a single-bond geometry to one Cu(1) and one C(21) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one Cu(2) and one C(21) atom. Linkers: 4 [O]C(=O)c1cc(cc(c1)C1=C2C=CC3=[N]2[Ni@]24n5c1ccc5C(=C1[N]2=C(C=C1)C(=c1n4c(=C3c2cc(cc(c2)C(=O)[O])C(=O)[O])cc1)c1cc(cc(c1)C(=O)[O])C(=O)[O])c1cc(cc(c1)C(=O)[O])C(=O)[O])C(=O)[O] ,4 [O]C(=O)C1=C[C@]23[C]4[C]([CH]1)[CH]C(C([O])=O)=C[C@@]42[C@]31c2ccc3n2[Ni]24n5c(ccc5[C@]5(c6ccc1n62)[C@]12C=C(C([O])=O)[CH][C]6[CH]C(C([O])=O)=C[C@@]15[C]62)C(c1cc(C([O])=O)cc(C([O])=O)c1)=c1ccc(n14)=C3c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 16 [C]1O[Cu]234O[C]O[Cu]2(O1)(O[C]O3)O[C]O4. RCSR code: scu. The MOF has largest included sphere 14.39 A, density 0.79 g/cm3, surface area 3544.64 m2/g, accessible volume 0.81 cm3/g