Ni2C48H38(N4O3)3(CH)8(C5H4O)2 crystallizes in the monoclinic C2/c space group. The structure is zero-dimensional and consists of thirty-two 02329_fluka molecules, eight 3-methoxy-2-methylprop-1-ene molecules, and four Ni2C48H38(N4O3)3 clusters. In each Ni2C48H38(N4O3)3 cluster, Ni(1) is bonded in a 7-coordinate geometry to one N(1), one N(4), one H(27), one O(1), one O(2), one O(3), and one O(4) atom. The Ni(1)-N(1) bond length is 2.10 Å. The Ni(1)-N(4) bond length is 2.09 Å. The Ni(1)-H(27) bond length is 2.11 Å. The Ni(1)-O(1) bond length is 2.11 Å. The Ni(1)-O(2) bond length is 2.01 Å. The Ni(1)-O(3) bond length is 2.10 Å. The Ni(1)-O(4) bond length is 2.02 Å. There are twenty-four inequivalent C sites. In the first C site, C(23) is bonded in a trigonal planar geometry to one C(19), one C(24), and one C(3) atom. The C(23)-C(19) bond length is 1.38 Å. The C(23)-C(24) bond length is 1.50 Å. The C(23)-C(3) bond length is 1.37 Å. In the second C site, C(24) is bonded in a trigonal planar geometry to one C(13), one C(23), and one C(33) atom. The C(24)-C(13) bond length is 1.40 Å. The C(24)-C(33) bond length is 1.39 Å. In the third C site, C(25) is bonded in a 3-coordinate geometry to one C(14), one N(3), one H(13), and one H(14) atom. The C(25)-C(14) bond length is 1.52 Å. The C(25)-N(3) bond length is 1.47 Å. The C(25)-H(13) bond length is 0.97 Å. The C(25)-H(14) bond length is 0.97 Å. In the fourth C site, C(28) is bonded in a single-bond geometry to one C(7) and one H(24) atom. The C(28)-C(7) bond length is 1.36 Å. The C(28)-H(24) bond length is 0.93 Å. In the fifth C site, C(29) is bonded in a distorted single-bond geometry to one C(13) and one H(16) atom. The C(29)-C(13) bond length is 1.40 Å. The C(29)-H(16) bond length is 0.93 Å. In the sixth C site, C(30) is bonded in a trigonal planar geometry to one C(10), one C(20), and one C(9) atom. The C(30)-C(10) bond length is 1.39 Å. The C(30)-C(20) bond length is 1.51 Å. The C(30)-C(9) bond length is 1.39 Å. In the seventh C site, C(32) is bonded in a distorted single-bond geometry to one C(14) and one H(6) atom. The C(32)-C(14) bond length is 1.38 Å. The C(32)-H(6) bond length is 0.93 Å. In the eighth C site, C(33) is bonded in a distorted single-bond geometry to one C(24) and one H(8,25) atom. The C(33)-H(8,25) bond length is 0.93 Å. In the ninth C site, C(1) is bonded in a trigonal planar geometry to one N(2), one N(4), and one H(4) atom. The C(1)-N(2) bond length is 1.31 Å. The C(1)-N(4) bond length is 1.33 Å. The C(1)-H(4) bond length is 0.93 Å. In the tenth C site, C(2) is bonded in a distorted single-bond geometry to one C(14) and one H(9) atom. The C(2)-C(14) bond length is 1.39 Å. The C(2)-H(9) bond length is 0.93 Å. In the eleventh C site, C(3) is bonded in a distorted single-bond geometry to one C(23) and one H(15) atom. The C(3)-H(15) bond length is 0.93 Å. In the twelfth C site, C(7) is bonded in a trigonal planar geometry to one C(15), one C(21), and one C(28) atom. The C(7)-C(15) bond length is 1.50 Å. The C(7)-C(21) bond length is 1.39 Å. In the thirteenth C site, C(9) is bonded in a distorted single-bond geometry to one C(30) and one H(22) atom. The C(9)-H(22) bond length is 0.93 Å. In the fourteenth C site, C(10) is bonded in a distorted single-bond geometry to one C(30) and one H(19) atom. The C(10)-H(19) bond length is 0.93 Å. In the fifteenth C site, C(13) is bonded in a trigonal planar geometry to one C(17), one C(24), and one C(29) atom. The C(13)-C(17) bond length is 1.51 Å. In the sixteenth C site, C(14) is bonded in a trigonal planar geometry to one C(2), one C(25), and one C(32) atom. In the seventeenth C site, C(15) is bonded in a 3-coordinate geometry to one C(7); one N(2); and two equivalent H(7,11) atoms. The C(15)-N(2) bond length is 1.47 Å. Both C(15)-H(7,11) bond lengths are 0.97 Å. In the eighteenth C site, C(16) is bonded in a trigonal planar geometry to one N(1), one N(3), and one H(10) atom. The C(16)-N(1) bond length is 1.31 Å. The C(16)-N(3) bond length is 1.31 Å. The C(16)-H(10) bond length is 0.93 Å. In the nineteenth C site, C(17) is bonded in a distorted bent 120 degrees geometry to one C(13), one O(1), and one O(2) atom. The C(17)-O(1) bond length is 1.25 Å. The C(17)-O(2) bond length is 1.25 Å. In the twentieth C site, C(18) is bonded in a trigonal planar geometry to one N(1), one N(5), and one H(18) atom. The C(18)-N(1) bond length is 1.33 Å. The C(18)-N(5) bond length is 1.29 Å. The C(18)-H(18) bond length is 0.93 Å. In the twenty-first C site, C(19) is bonded in a distorted single-bond geometry to one C(23) and one H(8,25) atom. The C(19)-H(8,25) bond length is 0.93 Å. In the twenty-second C site, C(20) is bonded in a distorted bent 120 degrees geometry to one C(30), one O(4), and one O(5) atom. The C(20)-O(4) bond length is 1.26 Å. The C(20)-O(5) bond length is 1.22 Å. In the twenty-third C site, C(21) is bonded in a single-bond geometry to one C(7) and one H(26) atom. The C(21)-H(26) bond length is 0.93 Å. In the twenty-fourth C site, C(22) is bonded in a trigonal planar geometry to one N(4), one N(6), and one H(5) atom. The C(22)-N(4) bond length is 1.35 Å. The C(22)-N(6) bond length is 1.30 Å. The C(22)-H(5) bond length is 0.93 Å. There are six inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Ni(1), one C(16), and one C(18) atom. In the second N site, N(3) is bonded in a 3-coordinate geometry to one C(16), one C(25), and one N(5) atom. The N(3)-N(5) bond length is 1.35 Å. In the third N site, N(2) is bonded in a 3-coordinate geometry to one C(1), one C(15), and one N(6) atom. The N(2)-N(6) bond length is 1.34 Å. In the fourth N site, N(5) is bonded in a distorted water-like geometry to one C(18) and one N(3) atom. In the fifth N site, N(4) is bonded in a distorted trigonal planar geometry to one Ni(1), one C(1), and one C(22) atom. In the sixth N site, N(6) is bonded in a water-like geometry to one C(22) and one N(2) atom. There are seventeen inequivalent H sites. In the first H site, H(4) is bonded in a single-bond geometry to one C(1) atom. In the second H site, H(5) is bonded in a single-bond geometry to one C(22) atom. In the third H site, H(6) is bonded in a single-bond geometry to one C(32) atom. In the fourth H site, H(7,11) is bonded in a single-bond geometry to one C(15) atom. In the fifth H site, H(8,25) is bonded in a single-bond geometry to one C(19) atom. In the sixth H site, H(9) is bonded in a single-bond geometry to one C(2) atom. In the seventh H site, H(10) is bonded in a single-bond geometry to one C(16) atom. In the eighth H site, H(13) is bonded in a single-bond geometry to one C(25) atom. In the ninth H site, H(14) is bonded in a single-bond geometry to one C(25) atom. In the tenth H site, H(15) is bonded in a single-bond geometry to one C(3) atom. In the eleventh H site, H(16) is bonded in a single-bond geometry to one C(29) atom. In the twelfth H site, H(18) is bonded in a single-bond geometry to one C(18) atom. In the thirteenth H site, H(19) is bonded in a single-bond geometry to one C(10) atom. In the fourteenth H site, H(22) is bonded in a single-bond geometry to one C(9) atom. In the fifteenth H site, H(24) is bonded in a single-bond geometry to one C(28) atom. In the sixteenth H site, H(26) is bonded in a single-bond geometry to one C(21) atom. In the seventeenth H site, H(27) is bonded in a single-bond geometry to one Ni(1) and one O(3) atom. The H(27)-O(3) bond length is 0.88 Å. There are five inequivalent O sites. In the first O site, O(1) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(17) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(17) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to two equivalent Ni(1) and two equivalent H(27) atoms. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(20) atom. In the fifth O site, O(5) is bonded in a single-bond geometry to one C(20) atom. Linkers: 3 [CH]1N=C[N]N1Cc1ccc(CN2[CH]N=C[N]2)cc1 ,4 [O]C(=O)c1cccc(OCc2ccc(-c3ccccc3C([O])=O)cc2)c1 ,2 [CH]1N=C[N]N1Cc1ccc(Cn2cncn2)cc1. Metal clusters: 2 O.O=[C]O[Ni]1O[C]O[Ni](O[C]=O)O[C]O1. The MOF has largest included sphere 5.23 A, density 1.22 g/cm3, surface area 5004.88 m2/g, accessible volume 0.27 cm3/g