Ni2C32N4H24O9(C4H3)2(C5H4)4 crystallizes in the monoclinic Cc space group. The structure consists of eight isobutylene molecules and eight naphthalene molecules inside a Ni2C32N4H24O9 framework. In the Ni2C32N4H24O9 framework, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one N(1), one N(3), one O(1), one O(4), one O(7), and one O(9) atom to form corner-sharing NiN2O4 octahedra. The corner-sharing octahedral tilt angles are 71°. The Ni(1)-N(1) bond length is 2.05 Å. The Ni(1)-N(3) bond length is 2.04 Å. The Ni(1)-O(1) bond length is 2.06 Å. The Ni(1)-O(4) bond length is 2.08 Å. The Ni(1)-O(7) bond length is 2.07 Å. The Ni(1)-O(9) bond length is 2.09 Å. In the second Ni site, Ni(2) is bonded to one N(2), one N(4), one O(2), one O(3), one O(8), and one O(9) atom to form corner-sharing NiN2O4 octahedra. The corner-sharing octahedral tilt angles are 71°. The Ni(2)-N(2) bond length is 2.05 Å. The Ni(2)-N(4) bond length is 2.04 Å. The Ni(2)-O(2) bond length is 2.06 Å. The Ni(2)-O(3) bond length is 2.08 Å. The Ni(2)-O(8) bond length is 2.07 Å. The Ni(2)-O(9) bond length is 2.09 Å. There are twenty-nine inequivalent C sites. In the first C site, C(33) is bonded in a trigonal planar geometry to one C(31,32); one C(35); and one C(37) atom. The C(33)-C(31,32) bond length is 1.40 Å. The C(33)-C(35) bond length is 1.40 Å. The C(33)-C(37) bond length is 1.51 Å. In the second C site, C(34) is bonded in a trigonal planar geometry to one C(31,32); one C(36); and one C(38) atom. The C(34)-C(31,32) bond length is 1.40 Å. The C(34)-C(36) bond length is 1.40 Å. The C(34)-C(38) bond length is 1.51 Å. In the third C site, C(35) is bonded in a distorted trigonal planar geometry to one C(25), one C(33), and one H(29) atom. The C(35)-C(25) bond length is 1.40 Å. The C(35)-H(29) bond length is 1.09 Å. In the fourth C site, C(36) is bonded in a distorted trigonal planar geometry to one C(26), one C(34), and one H(30) atom. The C(36)-C(26) bond length is 1.40 Å. The C(36)-H(30) bond length is 1.09 Å. In the fifth C site, C(37) is bonded in a distorted bent 120 degrees geometry to one C(33), one O(5), and one O(7) atom. The C(37)-O(5) bond length is 1.27 Å. The C(37)-O(7) bond length is 1.28 Å. In the sixth C site, C(38) is bonded in a distorted bent 120 degrees geometry to one C(34), one O(6), and one O(8) atom. The C(38)-O(6) bond length is 1.27 Å. The C(38)-O(8) bond length is 1.28 Å. In the seventh C site, C(39) is bonded in a distorted bent 120 degrees geometry to one C(25), one O(1), and one O(3) atom. The C(39)-C(25) bond length is 1.51 Å. The C(39)-O(1) bond length is 1.27 Å. The C(39)-O(3) bond length is 1.27 Å. In the eighth C site, C(40) is bonded in a distorted bent 120 degrees geometry to one C(26), one O(2), and one O(4) atom. The C(40)-C(26) bond length is 1.51 Å. The C(40)-O(2) bond length is 1.27 Å. The C(40)-O(4) bond length is 1.27 Å. In the ninth C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(3); one N(1); and one H(3,4) atom. The C(1)-C(3) bond length is 1.39 Å. The C(1)-N(1) bond length is 1.34 Å. The C(1)-H(3,4) bond length is 1.09 Å. In the tenth C site, C(2) is bonded in a distorted bent 120 degrees geometry to one C(4); one N(2); and one H(3,4) atom. The C(2)-C(4) bond length is 1.39 Å. The C(2)-N(2) bond length is 1.34 Å. The C(2)-H(3,4) bond length is 1.09 Å. In the eleventh C site, C(3) is bonded in a distorted trigonal planar geometry to one C(1); one C(5,6); and one H(5,6) atom. The C(3)-C(5,6) bond length is 1.40 Å. The C(3)-H(5,6) bond length is 1.09 Å. In the twelfth C site, C(4) is bonded in a distorted trigonal planar geometry to one C(2); one C(5,6); and one H(5,6) atom. The C(4)-C(5,6) bond length is 1.40 Å. The C(4)-H(5,6) bond length is 1.09 Å. In the thirteenth C site, C(5,6) is bonded in a trigonal planar geometry to one C(11); one C(3); and one C(7,8) atom. The C(5,6)-C(11) bond length is 1.49 Å. The C(5,6)-C(7,8) bond length is 1.40 Å. In the fourteenth C site, C(7,8) is bonded in a distorted single-bond geometry to one C(5,6) and one H(7,8) atom. The C(7,8)-H(7,8) bond length is 1.09 Å. In the fifteenth C site, C(9) is bonded in a distorted trigonal planar geometry to one N(1) and one H(9,10) atom. The C(9)-N(1) bond length is 1.35 Å. The C(9)-H(9,10) bond length is 1.09 Å. In the sixteenth C site, C(10) is bonded in a distorted trigonal planar geometry to one N(2) and one H(9,10) atom. The C(10)-N(2) bond length is 1.35 Å. The C(10)-H(9,10) bond length is 1.09 Å. In the seventeenth C site, C(11) is bonded in a single-bond geometry to one C(5,6) and one H(11,12) atom. The C(11)-H(11,12) bond length is 1.10 Å. In the eighteenth C site, C(12) is bonded in a single-bond geometry to one C(5,6) and one H(11,12) atom. The C(12)-C(5,6) bond length is 1.49 Å. The C(12)-H(11,12) bond length is 1.10 Å. In the nineteenth C site, C(19) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(17) atom. The C(19)-N(3) bond length is 1.34 Å. The C(19)-H(17) bond length is 1.09 Å. In the twentieth C site, C(20) is bonded in a distorted bent 120 degrees geometry to one N(4) and one H(18) atom. The C(20)-N(4) bond length is 1.34 Å. The C(20)-H(18) bond length is 1.09 Å. In the twenty-first C site, C(21) is bonded in a distorted bent 120 degrees geometry to one N(3) and one H(19) atom. The C(21)-N(3) bond length is 1.35 Å. The C(21)-H(19) bond length is 1.09 Å. In the twenty-second C site, C(22) is bonded in a distorted bent 120 degrees geometry to one N(4) and one H(20) atom. The C(22)-N(4) bond length is 1.35 Å. The C(22)-H(20) bond length is 1.09 Å. In the twenty-third C site, C(25) is bonded in a trigonal planar geometry to one C(27), one C(35), and one C(39) atom. The C(25)-C(27) bond length is 1.40 Å. In the twenty-fourth C site, C(26) is bonded in a trigonal planar geometry to one C(28), one C(36), and one C(40) atom. The C(26)-C(28) bond length is 1.40 Å. In the twenty-fifth C site, C(27) is bonded in a distorted single-bond geometry to one C(25); one C(29); and one H(23,24) atom. The C(27)-C(29) bond length is 1.40 Å. The C(27)-H(23,24) bond length is 1.09 Å. In the twenty-sixth C site, C(28) is bonded in a distorted single-bond geometry to one C(26); one C(30); and one H(23,24) atom. The C(28)-C(30) bond length is 1.40 Å. The C(28)-H(23,24) bond length is 1.09 Å. In the twenty-seventh C site, C(29) is bonded in a distorted trigonal planar geometry to one C(27); one C(31,32); and one H(25,26) atom. The C(29)-C(31,32) bond length is 1.39 Å. The C(29)-H(25,26) bond length is 1.09 Å. In the twenty-eighth C site, C(30) is bonded in a distorted trigonal planar geometry to one C(28); one C(31,32); and one H(25,26) atom. The C(30)-C(31,32) bond length is 1.39 Å. The C(30)-H(25,26) bond length is 1.09 Å. In the twenty-ninth C site, C(31,32) is bonded in a distorted trigonal planar geometry to one C(29), one C(33), and one H(27) atom. The C(31,32)-H(27) bond length is 1.09 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Ni(1), one C(1), and one C(9) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ni(2), one C(10), and one C(2) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Ni(1), one C(19), and one C(21) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one Ni(2), one C(20), and one C(22) atom. There are seventeen inequivalent H sites. In the first H site, H(1) is bonded in a distorted single-bond geometry to one O(6) and one O(9) atom. The H(1)-O(6) bond length is 1.55 Å. The H(1)-O(9) bond length is 1.04 Å. In the second H site, H(2) is bonded in a distorted single-bond geometry to one O(5) and one O(9) atom. The H(2)-O(5) bond length is 1.55 Å. The H(2)-O(9) bond length is 1.04 Å. In the third H site, H(3,4) is bonded in a single-bond geometry to one C(1) atom. In the fourth H site, H(5,6) is bonded in a single-bond geometry to one C(3) atom. In the fifth H site, H(7,8) is bonded in a single-bond geometry to one C(7,8) atom. In the sixth H site, H(9,10) is bonded in a single-bond geometry to one C(9) atom. In the seventh H site, H(11,12) is bonded in a single-bond geometry to one C(11) atom. In the eighth H site, H(17) is bonded in a single-bond geometry to one C(19) atom. In the ninth H site, H(18) is bonded in a single-bond geometry to one C(20) atom. In the tenth H site, H(19) is bonded in a single-bond geometry to one C(21) atom. In the eleventh H site, H(20) is bonded in a single-bond geometry to one C(22) atom. In the twelfth H site, H(23,24) is bonded in a single-bond geometry to one C(27) atom. In the thirteenth H site, H(25,26) is bonded in a single-bond geometry to one C(29) atom. In the fourteenth H site, H(27) is bonded in a single-bond geometry to one C(31,32) atom. In the fifteenth H site, H(28) is bonded in a single-bond geometry to one C(31,32) atom. The H(28)-C(31,32) bond length is 1.09 Å. In the sixteenth H site, H(29) is bonded in a single-bond geometry to one C(35) atom. In the seventeenth H site, H(30) is bonded in a single-bond geometry to one C(36) atom. There are nine inequivalent O sites. In the first O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(39) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(40) atom. In the third O site, O(3) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(39) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(40) atom. In the fifth O site, O(5) is bonded in a water-like geometry to one C(37) and one H(2) atom. In the sixth O site, O(6) is bonded in a water-like geometry to one C(38) and one H(1) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(37) atom. In the eighth O site, O(8) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(38) atom. In the ninth O site, O(9) is bonded in a distorted water-like geometry to one Ni(1), one Ni(2), one H(1), and one H(2) atom. Linkers: 4 [O]C(=O)c1cccc(C([O])=O)c1 ,2 c1cc([C@H]2[C@H](c3ccncc3)[C@@H](c3ccncc3)[C@@H]2c2ccncc2)ccn1. Metal clusters: 2 O.O=[C]O[Ni]1O[C]O[Ni](O[C]=O)O[C]O1. RCSR code: dia. The MOF has largest included sphere 4.46 A, density 1.26 g/cm3, surface area 4983.40 m2/g, accessible volume 0.25 cm3/g