Ni2C21N4H13O9(CH)3 crystallizes in the monoclinic P2_1/c space group. The structure consists of twelve 02329_fluka molecules inside a Ni2C21N4H13O9 framework. In the Ni2C21N4H13O9 framework, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one N(2), one N(4), one O(1), one O(3), one O(6), and one O(9) atom to form corner-sharing NiN2O4 octahedra. The corner-sharing octahedral tilt angles are 66°. The Ni(1)-N(2) bond length is 2.10 Å. The Ni(1)-N(4) bond length is 2.11 Å. The Ni(1)-O(1) bond length is 2.06 Å. The Ni(1)-O(3) bond length is 2.09 Å. The Ni(1)-O(6) bond length is 2.03 Å. The Ni(1)-O(9) bond length is 2.11 Å. In the second Ni site, Ni(2) is bonded to one N(1), one N(3), one O(4), one O(5), one O(8), and one O(9) atom to form corner-sharing NiN2O4 octahedra. The corner-sharing octahedral tilt angles are 66°. The Ni(2)-N(1) bond length is 2.10 Å. The Ni(2)-N(3) bond length is 2.08 Å. The Ni(2)-O(4) bond length is 2.02 Å. The Ni(2)-O(5) bond length is 2.10 Å. The Ni(2)-O(8) bond length is 2.08 Å. The Ni(2)-O(9) bond length is 2.13 Å. There are twenty-one 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(2) atom. The C(1)-C(2) bond length is 1.50 Å. The C(1)-O(1) bond length is 1.25 Å. The C(1)-O(2) 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(3), and one C(6) atom. The C(2)-C(3) bond length is 1.38 Å. The C(2)-C(6) bond length is 1.38 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2) and one H(1) atom. The C(3)-H(1) bond length is 0.93 Å. In the fourth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(3) atom. The C(5)-N(1) bond length is 1.33 Å. The C(5)-H(3) bond length is 0.93 Å. In the fifth C site, C(6) is bonded in a distorted bent 120 degrees geometry to one C(2), one N(1), and one H(4) atom. The C(6)-N(1) bond length is 1.34 Å. The C(6)-H(4) bond length is 0.93 Å. In the sixth C site, C(8) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(6) atom. The C(8)-N(2) bond length is 1.34 Å. The C(8)-H(6) bond length is 0.93 Å. In the seventh C site, C(9) is bonded in a 3-coordinate geometry to one C(11), one N(2), and one H(7) atom. The C(9)-C(11) bond length is 1.38 Å. The C(9)-N(2) bond length is 1.33 Å. The C(9)-H(7) bond length is 0.93 Å. In the eighth C site, C(10) is bonded in a distorted single-bond geometry to one C(11) and one H(8) atom. The C(10)-C(11) bond length is 1.38 Å. The C(10)-H(8) bond length is 0.93 Å. In the ninth C site, C(11) is bonded in a trigonal planar geometry to one C(10), one C(12), and one C(9) atom. The C(11)-C(12) bond length is 1.50 Å. In the tenth C site, C(12) is bonded in a distorted bent 120 degrees geometry to one C(11), one O(3), and one O(4) atom. The C(12)-O(3) bond length is 1.25 Å. The C(12)-O(4) bond length is 1.26 Å. In the eleventh C site, C(13) is bonded in a distorted bent 120 degrees geometry to one C(14), one O(5), and one O(6) atom. The C(13)-C(14) bond length is 1.50 Å. The C(13)-O(5) bond length is 1.26 Å. The C(13)-O(6) bond length is 1.25 Å. In the twelfth C site, C(14) is bonded in a trigonal planar geometry to one C(13), one C(15), and one C(18) atom. The C(14)-C(15) bond length is 1.39 Å. The C(14)-C(18) bond length is 1.38 Å. In the thirteenth C site, C(15) is bonded in a distorted single-bond geometry to one C(14) and one H(9) atom. The C(15)-H(9) bond length is 0.93 Å. In the fourteenth C site, C(16) is bonded in a distorted single-bond geometry to one C(17) and one H(10) atom. The C(16)-C(17) bond length is 1.37 Å. The C(16)-H(10) bond length is 0.93 Å. In the fifteenth C site, C(17) is bonded in a distorted trigonal planar geometry to one C(16), one N(3), and one H(11) atom. The C(17)-N(3) bond length is 1.34 Å. The C(17)-H(11) bond length is 0.93 Å. In the sixteenth C site, C(18) is bonded in a distorted bent 120 degrees geometry to one C(14), one N(3), and one H(12) atom. The C(18)-N(3) bond length is 1.34 Å. The C(18)-H(12) bond length is 0.93 Å. In the seventeenth C site, C(19) is bonded in a distorted bent 120 degrees geometry to one C(20), one O(7), and one O(8) atom. The C(19)-C(20) bond length is 1.51 Å. The C(19)-O(7) bond length is 1.25 Å. The C(19)-O(8) bond length is 1.26 Å. In the eighteenth C site, C(20) is bonded in a trigonal planar geometry to one C(19), one C(21), and one C(24) atom. The C(20)-C(21) bond length is 1.38 Å. The C(20)-C(24) bond length is 1.38 Å. In the nineteenth C site, C(21) is bonded in a distorted single-bond geometry to one C(20) and one H(13) atom. The C(21)-H(13) bond length is 0.93 Å. In the twentieth C site, C(23) is bonded in a distorted bent 120 degrees geometry to one N(4) and one H(15) atom. The C(23)-N(4) bond length is 1.34 Å. The C(23)-H(15) bond length is 0.93 Å. In the twenty-first C site, C(24) is bonded in a distorted bent 120 degrees geometry to one C(20), one N(4), and one H(16) atom. The C(24)-N(4) bond length is 1.34 Å. The C(24)-H(16) bond length is 0.93 Å. There are four inequivalent N sites. In the first N site, N(1) is bonded in a trigonal planar geometry to one Ni(2), one C(5), and one C(6) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ni(1), one C(8), and one C(9) atom. In the third N site, N(3) is bonded in a trigonal planar geometry to one Ni(2), one C(17), and one C(18) atom. In the fourth N site, N(4) is bonded in a trigonal planar geometry to one Ni(1), one C(23), and one C(24) atom. There are thirteen 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(3) is bonded in a single-bond geometry to one C(5) atom. In the third H site, H(4) is bonded in a single-bond geometry to one C(6) atom. In the fourth H site, H(6) is bonded in a single-bond geometry to one C(8) atom. In the fifth H site, H(7) is bonded in a single-bond geometry to one C(9) atom. In the sixth H site, H(8) is bonded in a single-bond geometry to one C(10) atom. In the seventh H site, H(9) is bonded in a single-bond geometry to one C(15) atom. In the eighth H site, H(10) is bonded in a single-bond geometry to one C(16) atom. In the ninth H site, H(11) is bonded in a single-bond geometry to one C(17) atom. In the tenth H site, H(12) is bonded in a single-bond geometry to one C(18) atom. In the eleventh H site, H(13) is bonded in a single-bond geometry to one C(21) atom. In the twelfth H site, H(15) is bonded in a single-bond geometry to one C(23) atom. In the thirteenth H site, H(16) is bonded in a single-bond geometry to one C(24) 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(1) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(1) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one Ni(1) and one C(12) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(12) atom. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(13) atom. In the sixth O site, O(6) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(13) atom. In the seventh O site, O(7) is bonded in a single-bond geometry to one C(19) atom. In the eighth O site, O(8) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(19) atom. In the ninth O site, O(9) is bonded in a bent 120 degrees geometry to one Ni(1) and one Ni(2) atom. Linkers: 16 [O]C(=O)c1cccnc1. Metal clusters: 4 O=[C]O[Ni@]12O[C]O[Ni@](O[C]=O)(O[C]O1)O2. The MOF has largest included sphere 4.16 A, density 1.47 g/cm3, surface area 4026.88 m2/g, accessible volume 0.27 cm3/g