Ni2C29N4H22O13(CH)2(CH2)3 crystallizes in the orthorhombic P2_12_12_1 space group. The structure consists of eight 02329_fluka molecules and twelve 02329_fluka molecules inside a Ni2C29N4H22O13 framework. In the Ni2C29N4H22O13 framework, there are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one N(1), one O(11), one O(12), one O(13), one O(2), and one O(3) atom to form corner-sharing NiNO5 octahedra. The corner-sharing octahedral tilt angles are 71°. The Ni(1)-N(1) bond length is 2.08 Å. The Ni(1)-O(11) bond length is 2.09 Å. The Ni(1)-O(12) bond length is 2.19 Å. The Ni(1)-O(13) bond length is 2.06 Å. The Ni(1)-O(2) bond length is 1.99 Å. The Ni(1)-O(3) bond length is 2.03 Å. In the second Ni site, Ni(2) is bonded to one N(2), one O(1), one O(10), one O(13), one O(4), and one O(7) atom to form corner-sharing NiNO5 octahedra. The corner-sharing octahedral tilt angles are 71°. The Ni(2)-N(2) bond length is 2.08 Å. The Ni(2)-O(1) bond length is 2.05 Å. The Ni(2)-O(10) bond length is 2.05 Å. The Ni(2)-O(13) bond length is 2.12 Å. The Ni(2)-O(4) bond length is 2.04 Å. The Ni(2)-O(7) bond length is 2.06 Å. There are twenty-nine inequivalent C sites. In the first C site, C(1) is bonded in a bent 120 degrees geometry to one C(2), one O(5), and one O(6) atom. The C(1)-C(2) bond length is 1.52 Å. The C(1)-O(5) bond length is 1.22 Å. The C(1)-O(6) 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(7) atom. The C(2)-C(3) bond length is 1.38 Å. The C(2)-C(7) bond length is 1.40 Å. In the third C site, C(3) is bonded in a distorted single-bond geometry to one C(2), one C(4), and one H(1) atom. The C(3)-C(4) bond length is 1.37 Å. The C(3)-H(1) bond length is 0.93 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(3), one C(5), and one C(6) atom. The C(4)-C(5) bond length is 1.50 Å. The C(4)-C(6) bond length is 1.41 Å. In the fifth C site, C(5) is bonded in a distorted bent 120 degrees geometry to one C(4), one O(3), and one O(4) atom. The C(5)-O(3) bond length is 1.27 Å. The C(5)-O(4) bond length is 1.23 Å. In the sixth C site, C(6) is bonded in a distorted single-bond geometry to one C(4), one C(8), and one H(2) atom. The C(6)-C(8) bond length is 1.36 Å. The C(6)-H(2) bond length is 0.93 Å. In the seventh C site, C(7) is bonded in a distorted single-bond geometry to one C(2), one C(8), and one H(3) atom. The C(7)-C(8) bond length is 1.41 Å. The C(7)-H(3) bond length is 0.93 Å. In the eighth C site, C(11) is bonded in a trigonal planar geometry to one C(10), one C(12), and one C(16) atom. The C(11)-C(10) bond length is 1.50 Å. The C(11)-C(12) bond length is 1.39 Å. The C(11)-C(16) bond length is 1.35 Å. In the ninth C site, C(13) is bonded in a trigonal planar geometry to one C(12), one C(14), and one C(17) atom. The C(13)-C(12) bond length is 1.39 Å. The C(13)-C(14) bond length is 1.37 Å. The C(13)-C(17) bond length is 1.54 Å. In the tenth C site, C(14) is bonded in a distorted single-bond geometry to one C(13), one C(15), and one H(5) atom. The C(14)-C(15) bond length is 1.41 Å. The C(14)-H(5) bond length is 0.93 Å. In the eleventh C site, C(15) is bonded in a trigonal planar geometry to one C(14), one C(16), and one C(18) atom. The C(15)-C(16) bond length is 1.40 Å. The C(15)-C(18) bond length is 1.47 Å. In the twelfth C site, C(16) is bonded in a distorted single-bond geometry to one C(11), one C(15), and one H(6) atom. The C(16)-H(6) bond length is 0.93 Å. In the thirteenth C site, C(17) is bonded in a distorted bent 120 degrees geometry to one C(13), one O(10), and one O(9) atom. The C(17)-O(10) bond length is 1.25 Å. The C(17)-O(9) bond length is 1.24 Å. In the fourteenth C site, C(18) is bonded in a bent 120 degrees geometry to one C(15), one O(11), and one O(12) atom. The C(18)-O(11) bond length is 1.25 Å. The C(18)-O(12) bond length is 1.29 Å. In the fifteenth C site, C(19) is bonded in a distorted bent 120 degrees geometry to one N(1) and one H(7) atom. The C(19)-N(1) bond length is 1.32 Å. The C(19)-H(7) bond length is 0.93 Å. In the sixteenth C site, C(21) is bonded in a distorted single-bond geometry to one C(22) and one H(9) atom. The C(21)-C(22) bond length is 1.34 Å. The C(21)-H(9) bond length is 0.93 Å. In the seventeenth C site, C(23) is bonded in a distorted trigonal planar geometry to one C(22), one N(1), and one H(10) atom. The C(23)-C(22) bond length is 1.38 Å. The C(23)-N(1) bond length is 1.34 Å. The C(23)-H(10) bond length is 0.93 Å. In the eighteenth C site, C(30) is bonded in a trigonal planar geometry to one C(29), one C(31), and one C(34) atom. The C(30)-C(29) bond length is 1.53 Å. The C(30)-C(31) bond length is 1.37 Å. The C(30)-C(34) bond length is 1.37 Å. In the nineteenth C site, C(31) is bonded in a distorted single-bond geometry to one C(30) and one H(23) atom. The C(31)-H(23) bond length is 0.93 Å. In the twentieth C site, C(8) is bonded in a trigonal planar geometry to one C(6), one C(7), and one C(9) atom. The C(8)-C(9) bond length is 1.53 Å. In the twenty-first C site, C(33) is bonded in a distorted bent 120 degrees geometry to one N(2) and one H(25) atom. The C(33)-N(2) bond length is 1.32 Å. The C(33)-H(25) bond length is 0.93 Å. In the twenty-second C site, C(34) is bonded in a 2-coordinate geometry to one C(30), one N(2), and one H(26) atom. The C(34)-N(2) bond length is 1.35 Å. The C(34)-H(26) bond length is 0.93 Å. In the twenty-third C site, C(9) is bonded in a distorted bent 120 degrees geometry to one C(8), one O(1), and one O(2) atom. The C(9)-O(1) bond length is 1.27 Å. The C(9)-O(2) bond length is 1.25 Å. In the twenty-fourth C site, C(10) is bonded in a bent 120 degrees geometry to one C(11), one O(7), and one O(8) atom. The C(10)-O(7) bond length is 1.25 Å. The C(10)-O(8) bond length is 1.26 Å. In the twenty-fifth C site, C(12) is bonded in a distorted single-bond geometry to one C(11), one C(13), and one H(4) atom. The C(12)-H(4) bond length is 0.93 Å. In the twenty-sixth C site, C(29) is bonded in a 3-coordinate geometry to one C(30); one N(4); and two equivalent H(21,22) atoms. The C(29)-N(4) bond length is 1.47 Å. Both C(29)-H(21,22) bond lengths are 0.97 Å. In the twenty-seventh C site, C(22) is bonded in a trigonal planar geometry to one C(21), one C(23), and one C(24) atom. The C(22)-C(24) bond length is 1.50 Å. In the twenty-eighth C site, C(24) is bonded in a 2-coordinate geometry to one C(22); one N(3); and two equivalent H(11,12) atoms. The C(24)-N(3) bond length is 1.48 Å. Both C(24)-H(11,12) bond lengths are 0.97 Å. In the twenty-ninth C site, C(25) is bonded in a distorted trigonal non-coplanar geometry to one N(3) and two equivalent H(13,14) atoms. The C(25)-N(3) bond length is 1.44 Å. Both C(25)-H(13,14) bond lengths are 0.97 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(19), and one C(23) atom. In the second N site, N(2) is bonded in a trigonal planar geometry to one Ni(2), one C(33), and one C(34) atom. In the third N site, N(3) is bonded in a distorted water-like geometry to one C(24), one C(25), one H(27), and one H(28) atom. The N(3)-H(27) bond length is 0.87 Å. The N(3)-H(28) bond length is 0.89 Å. In the fourth N site, N(4) is bonded in a distorted water-like geometry to one C(29), one H(29), and one H(30) atom. The N(4)-H(29) bond length is 0.86 Å. The N(4)-H(30) bond length is 0.85 Å. There are nineteen 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(6) atom. In the third H site, H(3) is bonded in a single-bond geometry to one C(7) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one C(12) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one C(14) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one C(16) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(19) atom. In the eighth H site, H(9) is bonded in a single-bond geometry to one C(21) atom. In the ninth H site, H(10) is bonded in a single-bond geometry to one C(23) atom. In the tenth H site, H(11,12) is bonded in a single-bond geometry to one C(24) atom. In the eleventh H site, H(13,14) is bonded in a single-bond geometry to one C(25) atom. In the twelfth H site, H(21,22) is bonded in a single-bond geometry to one C(29) atom. In the thirteenth H site, H(23) is bonded in a single-bond geometry to one C(31) atom. In the fourteenth H site, H(25) is bonded in a single-bond geometry to one C(33) atom. In the fifteenth H site, H(26) is bonded in a single-bond geometry to one C(34) atom. In the sixteenth H site, H(27) is bonded in a single-bond geometry to one N(3) atom. In the seventeenth H site, H(28) is bonded in a single-bond geometry to one N(3) atom. In the eighteenth H site, H(29) is bonded in a single-bond geometry to one N(4) atom. In the nineteenth H site, H(30) is bonded in a single-bond geometry to one N(4) atom. There are thirteen inequivalent O sites. In the first O site, O(8) is bonded in a single-bond geometry to one C(10) atom. In the second O site, O(9) is bonded in a single-bond geometry to one C(17) atom. In the third O site, O(10) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(17) atom. In the fourth O site, O(11) is bonded in an L-shaped geometry to one Ni(1) and one C(18) atom. In the fifth O site, O(3) is bonded in a bent 120 degrees geometry to one Ni(1) and one C(5) atom. In the sixth O site, O(12) is bonded in an L-shaped geometry to one Ni(1) and one C(18) atom. In the seventh O site, O(13) is bonded in a water-like geometry to one Ni(1) and one Ni(2) atom. In the eighth O site, O(1) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(9) atom. In the ninth O site, O(2) is bonded in a distorted bent 150 degrees geometry to one Ni(1) and one C(9) atom. In the tenth O site, O(7) is bonded in a distorted bent 120 degrees geometry to one Ni(2) and one C(10) atom. In the eleventh O site, O(4) is bonded in a bent 120 degrees geometry to one Ni(2) and one C(5) atom. In the twelfth O site, O(6) is bonded in a single-bond geometry to one C(1) atom. In the thirteenth O site, O(5) is bonded in a single-bond geometry to one C(1) atom. Linkers: 8 [O]C(=O)c1cc(C([O])=O)cc(C([O])=O)c1 ,4 C([NH2]Cc1cccnc1)CCC[NH2]Cc1cccnc1. Metal clusters: 4 O=[C]O[Ni]12(O[C]=O)O[C]O[Ni]3(O[C]O3)(O[C]O1)O2. The MOF has largest included sphere 5.07 A, density 1.25 g/cm3, surface area 4314.68 m2/g, accessible volume 0.31 cm3/g