Ni3C22H12(NO7)2(C3H2)2 crystallizes in the monoclinic P2_1/c space group. The structure consists of two 2,3-dimethyl-1,3-butadiene molecules inside a Ni3C22H12(NO7)2 framework. In the Ni3C22H12(NO7)2 framework, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded in a rectangular see-saw-like geometry to one O(1), one O(2), one O(3), and one O(4) atom. The Ni(1)-O(1) bond length is 2.02 Å. The Ni(1)-O(2) bond length is 2.09 Å. The Ni(1)-O(3) bond length is 2.07 Å. The Ni(1)-O(4) bond length is 2.01 Å. In the second Ni site, Ni(2) is bonded in an octahedral geometry to two equivalent O(2), two equivalent O(5), and two equivalent O(6) atoms. Both Ni(2)-O(2) bond lengths are 2.17 Å. Both Ni(2)-O(5) bond lengths are 1.98 Å. Both Ni(2)-O(6) bond lengths are 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 C(2), one O(1), and one O(5) atom. The C(1)-C(2) bond length is 1.51 Å. The C(1)-O(1) bond length is 1.26 Å. The C(1)-O(5) bond length is 1.25 Å. In the second C site, C(2) is bonded in a trigonal planar geometry to one C(1), one C(5), and one C(6) atom. The C(2)-C(5) bond length is 1.38 Å. The C(2)-C(6) bond length is 1.40 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(1) atom. The C(3)-N(1) bond length is 1.34 Å. The C(3)-H(1) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(2) atom. The C(4)-N(1) bond length is 1.33 Å. The C(4)-H(2) bond length is 0.93 Å. In the fifth C site, C(5) is bonded in a single-bond geometry to one C(2), one C(9), and one H(3) atom. The C(5)-C(9) bond length is 1.39 Å. The C(5)-H(3) bond length is 0.93 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(10), one C(2), and one H(4) atom. The C(6)-C(10) bond length is 1.39 Å. The C(6)-H(4) bond length is 0.93 Å. In the seventh C site, C(9) is bonded in a trigonal planar geometry to one C(12), one C(13), and one C(5) atom. The C(9)-C(12) bond length is 1.39 Å. The C(9)-C(13) bond length is 1.52 Å. In the eighth C site, C(10) is bonded in a trigonal planar geometry to one C(12), one C(14), and one C(6) atom. The C(10)-C(12) bond length is 1.40 Å. The C(10)-C(14) bond length is 1.50 Å. In the ninth C site, C(12) is bonded in a distorted single-bond geometry to one C(10), one C(9), and one H(7) atom. The C(12)-H(7) bond length is 0.93 Å. In the tenth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(9), one O(3), and one O(7) atom. The C(13)-O(3) bond length is 1.26 Å. The C(13)-O(7) bond length is 1.25 Å. In the eleventh C site, C(14) is bonded in a distorted bent 120 degrees geometry to one C(10), one O(4), and one O(6) atom. The C(14)-O(4) bond length is 1.25 Å. The C(14)-O(6) bond length is 1.26 Å. N(1) is bonded in a trigonal planar geometry to one C(3), one C(4), and one O(2) atom. The N(1)-O(2) bond length is 1.38 Å. There are six inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one C(3) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(4) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(5) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(6) atom. In the fifth H site, H(7) is bonded in a single-bond geometry to one C(12) atom. In the sixth H site, H(8) is bonded in a single-bond geometry to one O(2) atom. The H(8)-O(2) bond length is 0.98 Å. There are seven 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(1) atom. In the second O site, O(2) is bonded in a distorted single-bond geometry to one Ni(1), one Ni(2), one N(1), and one H(8) atom. In the third O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(13) atom. In the fourth O site, O(4) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one C(14) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(1) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(14) atom. In the seventh O site, O(7) is bonded in a single-bond geometry to one C(13) atom. Linkers: 3 ON1[CH]C=C(C2=C[CH]N(O)C=C2)C=C1 ,4 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1. Metal clusters: 2 O=[C]O[Ni@]1(O)O[C]O[Ni]2(O[C]O[Ni@@](O)(O[C]=O)O[C]O2)O[C]O1. The MOF has largest included sphere 5.24 A, density 1.29 g/cm3, surface area 3533.13 m2/g, accessible volume 0.38 cm3/g