Ni2C22N4H16O9(C4H3)4(CH)2 crystallizes in the orthorhombic Fdd2 space group. The structure consists of sixteen 02329_fluka molecules and thirty-two isobutylene molecules inside a Ni2C22N4H16O9 framework. In the Ni2C22N4H16O9 framework, Ni(1) is bonded in a 6-coordinate geometry to one N(1), one N(2), one O(1), one O(2), one O(4), and one O(5) atom. The Ni(1)-N(1) bond length is 2.09 Å. The Ni(1)-N(2) bond length is 2.10 Å. The Ni(1)-O(1) bond length is 2.06 Å. The Ni(1)-O(2) bond length is 2.05 Å. The Ni(1)-O(4) bond length is 2.06 Å. The Ni(1)-O(5) bond length is 2.10 Å. There are eleven inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(2) atom. The C(1)-N(1) bond length is 1.34 Å. The C(1)-H(2) bond length is 0.94 Å. In the second C site, C(5) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(5) atom. The C(5)-N(1) bond length is 1.34 Å. The C(5)-H(5) bond length is 0.94 Å. In the third C site, C(10) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(9) atom. The C(10)-N(2) bond length is 1.36 Å. The C(10)-H(9) bond length is 0.94 Å. In the fourth C site, C(11) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(10) atom. The C(11)-N(2) bond length is 1.31 Å. The C(11)-H(10) bond length is 0.94 Å. In the fifth C site, C(13) is bonded in a trigonal planar geometry to one C(14), one C(18), and one C(19) atom. The C(13)-C(14) bond length is 1.39 Å. The C(13)-C(18) bond length is 1.42 Å. The C(13)-C(19) bond length is 1.53 Å. In the sixth C site, C(14) is bonded in a distorted single-bond geometry to one C(13) and one H(12) atom. The C(14)-H(12) bond length is 0.94 Å. In the seventh C site, C(16) is bonded in a single-bond geometry to one C(17) and one H(14) atom. The C(16)-C(17) bond length is 1.43 Å. The C(16)-H(14) bond length is 0.94 Å. In the eighth C site, C(17) is bonded in a trigonal planar geometry to one C(16), one C(18), and one C(20) atom. The C(17)-C(18) bond length is 1.37 Å. The C(17)-C(20) bond length is 1.54 Å. In the ninth C site, C(18) is bonded in a distorted single-bond geometry to one C(13), one C(17), and one H(15) atom. The C(18)-H(15) bond length is 0.94 Å. In the tenth C site, C(19) is bonded in a bent 120 degrees geometry to one C(13), one O(1), and one O(2) atom. The C(19)-O(1) bond length is 1.25 Å. The C(19)-O(2) bond length is 1.28 Å. In the eleventh C site, C(20) is bonded in a distorted bent 120 degrees geometry to one C(17), one O(3), and one O(4) atom. The C(20)-O(3) bond length is 1.24 Å. The C(20)-O(4) bond length is 1.30 Å. There are two 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(5) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ni(1), one C(10), and one C(11) atom. There are eight inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(5) atom. The H(1)-O(5) bond length is 0.80 Å. In the second H site, H(2) is bonded in a single-bond geometry to one C(1) atom. In the third H site, H(5) is bonded in a single-bond geometry to one C(5) atom. In the fourth H site, H(9) is bonded in a single-bond geometry to one C(10) atom. In the fifth H site, H(10) is bonded in a single-bond geometry to one C(11) atom. In the sixth H site, H(12) is bonded in a single-bond geometry to one C(14) atom. In the seventh H site, H(14) is bonded in a single-bond geometry to one C(16) atom. In the eighth H site, H(15) is bonded in a single-bond geometry to one C(18) atom. 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(19) atom. In the second O site, O(2) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(19) atom. In the third O site, O(3) is bonded in a single-bond geometry to one C(20) atom. 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 distorted bent 120 degrees geometry to two equivalent Ni(1) and two equivalent H(1) atoms. Linkers: 2 c1cc([C@H]2[C@H](c3ccncc3)[C@@H](c3ccncc3)[C@@H]2c2ccncc2)ccn1 ,4 [O]C(=O)c1cccc(C([O])=O)c1. 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 6.46 A, density 0.93 g/cm3, surface area 4358.19 m2/g, accessible volume 0.56 cm3/g