NiC24H16(NO)4(CH)2 crystallizes in the triclinic P-1 space group. The structure consists of four 02329_fluka molecules inside a NiC24H16(NO)4 framework. In the NiC24H16(NO)4 framework, Ni(1) is bonded in a distorted octahedral geometry to one N(1), one N(2), one O(1), one O(2), one O(3), and one O(4) atom. The Ni(1)-N(1) bond length is 2.05 Å. The Ni(1)-N(2) bond length is 2.05 Å. The Ni(1)-O(1) bond length is 2.23 Å. The Ni(1)-O(2) bond length is 2.17 Å. The Ni(1)-O(3) bond length is 2.02 Å. The Ni(1)-O(4) bond length is 2.03 Å. There are twenty-four 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(1) atom. The C(1)-N(1) bond length is 1.35 Å. The C(1)-H(1) bond length is 1.09 Å. In the second C site, C(2) is bonded in a distorted single-bond geometry to one C(3) and one H(2) atom. The C(2)-C(3) bond length is 1.41 Å. The C(2)-H(2) bond length is 1.09 Å. In the third 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 1.41 Å. The C(3)-C(6) bond length is 1.46 Å. In the fourth C site, C(4) is bonded in a distorted single-bond geometry to one C(3), one C(5), and one H(3) atom. The C(4)-C(5) bond length is 1.39 Å. The C(4)-H(3) bond length is 1.09 Å. In the fifth C site, C(5) is bonded in a distorted trigonal planar geometry to one C(4), one N(1), and one H(4) atom. The C(5)-N(1) bond length is 1.34 Å. The C(5)-H(4) bond length is 1.09 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(3), one C(7), and one H(5) atom. The C(6)-C(7) bond length is 1.35 Å. The C(6)-H(5) bond length is 1.09 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(6), one C(8), and one H(6) atom. The C(7)-C(8) bond length is 1.45 Å. The C(7)-H(6) bond length is 1.09 Å. In the eighth 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 1.41 Å. The C(8)-C(9) bond length is 1.41 Å. In the ninth C site, C(9) is bonded in a distorted single-bond geometry to one C(8) and one H(7) atom. The C(9)-H(7) bond length is 1.09 Å. In the tenth C site, C(10) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(8) atom. The C(10)-N(2) bond length is 1.34 Å. The C(10)-H(8) bond length is 1.09 Å. In the eleventh C site, C(11) is bonded in a distorted bent 120 degrees geometry to one C(12), one N(2), and one H(9) atom. The C(11)-C(12) bond length is 1.38 Å. The C(11)-N(2) bond length is 1.35 Å. The C(11)-H(9) bond length is 1.09 Å. In the twelfth C site, C(12) is bonded in a distorted trigonal planar geometry to one C(11), one C(8), and one H(10) atom. The C(12)-H(10) bond length is 1.09 Å. In the thirteenth C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(14), one O(3), and one O(4) atom. The C(13)-C(14) bond length is 1.50 Å. The C(13)-O(3) bond length is 1.27 Å. The C(13)-O(4) bond length is 1.27 Å. In the fourteenth C site, C(14) is bonded in a trigonal planar geometry to one C(13), one C(15), and one C(19) atom. The C(14)-C(15) bond length is 1.40 Å. The C(14)-C(19) bond length is 1.40 Å. In the fifteenth C site, C(15) is bonded in a distorted single-bond geometry to one C(14) and one H(11) atom. The C(15)-H(11) bond length is 1.09 Å. In the sixteenth C site, C(17) is bonded in a distorted single-bond geometry to one C(18) and one H(13) atom. The C(17)-C(18) bond length is 1.41 Å. The C(17)-H(13) bond length is 1.09 Å. In the seventeenth C site, C(18) is bonded in a distorted trigonal planar geometry to one C(17), one C(19), and one N(3) atom. The C(18)-C(19) bond length is 1.40 Å. The C(18)-N(3) bond length is 1.41 Å. In the eighteenth C site, C(19) is bonded in a distorted single-bond geometry to one C(14), one C(18), and one H(14) atom. The C(19)-H(14) bond length is 1.09 Å. In the nineteenth C site, C(20) is bonded in a distorted bent 120 degrees geometry to one C(21), one O(1), and one O(2) atom. The C(20)-C(21) bond length is 1.49 Å. The C(20)-O(1) bond length is 1.28 Å. The C(20)-O(2) bond length is 1.28 Å. In the twentieth C site, C(21) is bonded in a trigonal planar geometry to one C(20), one C(22), and one C(26) atom. The C(21)-C(22) bond length is 1.40 Å. The C(21)-C(26) bond length is 1.40 Å. In the twenty-first C site, C(22) is bonded in a distorted single-bond geometry to one C(21) and one H(15) atom. The C(22)-H(15) bond length is 1.09 Å. In the twenty-second C site, C(24) is bonded in a distorted single-bond geometry to one C(25) and one H(17) atom. The C(24)-C(25) bond length is 1.41 Å. The C(24)-H(17) bond length is 1.09 Å. In the twenty-third 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 1.40 Å. The C(25)-N(4) bond length is 1.42 Å. In the twenty-fourth C site, C(26) is bonded in a distorted single-bond geometry to one C(21), one C(25), and one H(18) atom. The C(26)-H(18) 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(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. In the third N site, N(3) is bonded in a distorted bent 120 degrees geometry to one C(18) and one N(3) atom. The N(3)-N(3) bond length is 1.27 Å. In the fourth N site, N(4) is bonded in a distorted bent 120 degrees geometry to one C(25) and one N(4) atom. The N(4)-N(4) bond length is 1.27 Å. There are sixteen 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(2) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(4) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(5) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(6) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(7) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(9) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(10) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(11) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(12) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(15) atom. In the twelfth H site, H(13) is bonded in a single-bond geometry to one C(17) atom. In the thirteenth H site, H(14) is bonded in a single-bond geometry to one C(19) atom. In the fourteenth H site, H(15) is bonded in a single-bond geometry to one C(22) atom. In the fifteenth H site, H(17) is bonded in a single-bond geometry to one C(24) atom. In the sixteenth H site, H(18) is bonded in a single-bond geometry to one C(26) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a distorted L-shaped geometry to one Ni(1) and one C(20) atom. In the second O site, O(2) is bonded in a distorted L-shaped geometry to one Ni(1) and one C(20) atom. In the third O site, O(3) is bonded in a distorted bent 150 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(13) atom. Linkers: 2 [O]C(=O)c1cccc([N][N]c2cccc([C]=O)c2)c1 ,2 [O]C(=O)c1cccc([N][N]c2cccc(C([O])=O)c2)c1 ,2 C(=C/c1ccncc1)\c1ccncc1. Metal clusters: 1 [C]1O[Ni]2(O1)O[C]O[Ni]1(O[C]O1)O[C]O2. The MOF has largest included sphere 2.38 A, density 1.48 g/cm3, surface area 4875.55 m2/g, accessible volume 0.20 cm3/g