FeNi2C30H44(N9O2)2CO crystallizes in the monoclinic C2/c space group. The structure consists of eight methanol molecules inside a FeNi2C30H44(N9O2)2 framework. In the FeNi2C30H44(N9O2)2 framework, Fe(1) is bonded in an octahedral geometry to one C(1), one C(2), one C(3), one C(4), one C(5), and one C(6) atom. The Fe(1)-C(1) bond length is 1.90 Å. The Fe(1)-C(2) bond length is 1.91 Å. The Fe(1)-C(3) bond length is 1.90 Å. The Fe(1)-C(4) bond length is 1.91 Å. The Fe(1)-C(5) bond length is 1.90 Å. The Fe(1)-C(6) bond length is 1.89 Å. There are three inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one N(10), one N(11), one N(12), one N(4), one N(6), and one N(9) atom to form NiN6 octahedra that share  a cornercorner with one C(11)H2N2 tetrahedra,  a cornercorner with one C(14)H2N2 tetrahedra,  a cornercorner with one C(15)H2N2 tetrahedra, and  a cornercorner with one C(18)H2N2 tetrahedra. The Ni(1)-N(10) bond length is 2.13 Å. The Ni(1)-N(11) bond length is 2.05 Å. The Ni(1)-N(12) bond length is 2.07 Å. The Ni(1)-N(4) bond length is 2.10 Å. The Ni(1)-N(6) bond length is 2.11 Å. The Ni(1)-N(9) bond length is 2.09 Å. In the second Ni site, Ni(2) is bonded to two equivalent N(3), two equivalent N(7), and two equivalent N(8) atoms to form NiN6 octahedra that share corners with two equivalent C(10)H2N2 tetrahedra and corners with two equivalent C(9)H2N2 tetrahedra. Both Ni(2)-N(3) bond lengths are 2.11 Å. Both Ni(2)-N(7) bond lengths are 2.05 Å. Both Ni(2)-N(8) bond lengths are 2.06 Å. In the third Ni site, Ni(3) is bonded to two equivalent N(13), two equivalent N(14), and two equivalent N(5) atoms to form NiN6 octahedra that share corners with two equivalent C(21)H2N2 tetrahedra and corners with two equivalent C(22)H2N2 tetrahedra. Both Ni(3)-N(13) bond lengths are 2.10 Å. Both Ni(3)-N(14) bond lengths are 2.05 Å. Both Ni(3)-N(5) bond lengths are 2.11 Å. There are thirty inequivalent C sites. In the first C site, C(1) is bonded in a linear geometry to one Fe(1) and one N(4) atom. The C(1)-N(4) bond length is 1.15 Å. In the second C site, C(2) is bonded in a linear geometry to one Fe(1) and one N(1) atom. The C(2)-N(1) bond length is 1.16 Å. In the third C site, C(3) is bonded in a linear geometry to one Fe(1) and one N(5) atom. The C(3)-N(5) bond length is 1.14 Å. In the fourth C site, C(4) is bonded in a linear geometry to one Fe(1) and one N(2) atom. The C(4)-N(2) bond length is 1.15 Å. In the fifth C site, C(5) is bonded in a linear geometry to one Fe(1) and one N(3) atom. The C(5)-N(3) bond length is 1.16 Å. In the sixth C site, C(6) is bonded in a linear geometry to one Fe(1) and one N(6) atom. The C(6)-N(6) bond length is 1.15 Å. In the seventh C site, C(7) is bonded in a 3-coordinate geometry to one C(8), one N(8), one H(7), and one H(8) atom. The C(7)-C(8) bond length is 1.47 Å. The C(7)-N(8) bond length is 1.47 Å. The C(7)-H(7) bond length is 0.96 Å. The C(7)-H(8) bond length is 0.96 Å. In the eighth C site, C(8) is bonded in a 4-coordinate geometry to one C(7), one N(7), one H(10), and one H(9) atom. The C(8)-N(7) bond length is 1.50 Å. The C(8)-H(10) bond length is 0.96 Å. The C(8)-H(9) bond length is 0.96 Å. In the ninth C site, C(9) is bonded to one N(16), one N(8), one H(11), and one H(12) atom to form CH2N2 tetrahedra that share  a cornercorner with one Ni(2)N6 octahedra and  a cornercorner with one C(10)H2N2 tetrahedra. The corner-sharing octahedral tilt angles are 67°. The C(9)-N(16) bond length is 1.43 Å. The C(9)-N(8) bond length is 1.50 Å. The C(9)-H(11) bond length is 0.96 Å. The C(9)-H(12) bond length is 0.96 Å. In the tenth C site, C(10) is bonded to one N(16), one N(7), one H(13), and one H(14) atom to form CH2N2 tetrahedra that share  a cornercorner with one Ni(2)N6 octahedra and  a cornercorner with one C(9)H2N2 tetrahedra. The corner-sharing octahedral tilt angles are 65°. The C(10)-N(16) bond length is 1.43 Å. The C(10)-N(7) bond length is 1.48 Å. The C(10)-H(13) bond length is 0.96 Å. The C(10)-H(14) bond length is 0.96 Å. In the eleventh C site, C(11) is bonded to one N(10), one N(17), one H(15), and one H(16) atom to form CH2N2 tetrahedra that share  a cornercorner with one Ni(1)N6 octahedra and  a cornercorner with one C(18)H2N2 tetrahedra. The corner-sharing octahedral tilt angles are 68°. The C(11)-N(10) bond length is 1.51 Å. The C(11)-N(17) bond length is 1.39 Å. The C(11)-H(15) bond length is 0.96 Å. The C(11)-H(16) bond length is 0.96 Å. In the twelfth C site, C(12) is bonded in a 2-coordinate geometry to one C(13), one H(17), and one H(18) atom. The C(12)-C(13) bond length is 1.34 Å. The C(12)-H(17) bond length is 0.96 Å. The C(12)-H(18) bond length is 0.96 Å. In the thirteenth C site, C(13) is bonded in a 4-coordinate geometry to one C(12), one N(12), one H(19), and one H(20) atom. The C(13)-N(12) bond length is 1.56 Å. The C(13)-H(19) bond length is 0.96 Å. The C(13)-H(20) bond length is 0.96 Å. In the fourteenth C site, C(14) is bonded to one N(12), one N(18), one H(21), and one H(22) atom to form CH2N2 tetrahedra that share  a cornercorner with one Ni(1)N6 octahedra and  a cornercorner with one C(15)H2N2 tetrahedra. The corner-sharing octahedral tilt angles are 68°. The C(14)-N(12) bond length is 1.38 Å. The C(14)-N(18) bond length is 1.50 Å. The C(14)-H(21) bond length is 0.96 Å. The C(14)-H(22) bond length is 0.96 Å. In the fifteenth C site, C(15) is bonded to one N(18), one N(9), one H(23), and one H(24) atom to form distorted CH2N2 tetrahedra that share  a cornercorner with one Ni(1)N6 octahedra and  a cornercorner with one C(14)H2N2 tetrahedra. The corner-sharing octahedral tilt angles are 83°. The C(15)-N(18) bond length is 1.42 Å. The C(15)-N(9) bond length is 1.28 Å. The C(15)-H(23) bond length is 0.96 Å. The C(15)-H(24) bond length is 0.96 Å. In the sixteenth C site, C(16) is bonded in a 4-coordinate geometry to one C(17), one N(9), one H(25), and one H(26) atom. The C(16)-C(17) bond length is 1.31 Å. The C(16)-N(9) bond length is 1.41 Å. The C(16)-H(25) bond length is 0.96 Å. The C(16)-H(26) bond length is 0.96 Å. In the seventeenth C site, C(17) is bonded in a 2-coordinate geometry to one C(16), one H(27), and one H(28) atom. The C(17)-H(27) bond length is 0.96 Å. The C(17)-H(28) bond length is 0.96 Å. In the eighteenth C site, C(18) is bonded to one N(11), one N(17), one H(29), and one H(30) atom to form distorted CH2N2 tetrahedra that share  a cornercorner with one Ni(1)N6 octahedra and  a cornercorner with one C(11)H2N2 tetrahedra. The corner-sharing octahedral tilt angles are 62°. The C(18)-N(11) bond length is 1.29 Å. The C(18)-N(17) bond length is 1.57 Å. The C(18)-H(29) bond length is 0.96 Å. The C(18)-H(30) bond length is 0.96 Å. In the nineteenth C site, C(19) is bonded in a 4-coordinate geometry to one C(19), one N(13), one H(32), and one H(33) atom. The C(19)-C(19) bond length is 1.43 Å. The C(19)-N(13) bond length is 1.43 Å. The C(19)-H(32) bond length is 0.96 Å. The C(19)-H(33) bond length is 0.96 Å. In the twentieth C site, C(20) is bonded in a distorted trigonal non-coplanar geometry to one N(14), one H(35), and one H(36) atom. The C(20)-N(14) bond length is 1.40 Å. The C(20)-H(35) bond length is 0.96 Å. The C(20)-H(36) bond length is 0.96 Å. In the twenty-first C site, C(21) is bonded to one N(14), one N(15), one H(37), and one H(38) atom to form distorted CH2N2 tetrahedra that share  a cornercorner with one Ni(3)N6 octahedra and  a cornercorner with one C(22)H2N2 tetrahedra. The corner-sharing octahedral tilt angles are 67°. The C(21)-N(14) bond length is 1.56 Å. The C(21)-N(15) bond length is 1.39 Å. The C(21)-H(37) bond length is 0.96 Å. The C(21)-H(38) bond length is 0.96 Å. In the twenty-second C site, C(22) is bonded to one N(13), one N(15), one H(39), and one H(40) atom to form CH2N2 tetrahedra that share  a cornercorner with one Ni(3)N6 octahedra and  a cornercorner with one C(21)H2N2 tetrahedra. The corner-sharing octahedral tilt angles are 65°. The C(22)-N(13) bond length is 1.48 Å. The C(22)-N(15) bond length is 1.35 Å. The C(22)-H(39) bond length is 0.96 Å. The C(22)-H(40) bond length is 0.96 Å. In the twenty-third C site, C(23) is bonded in a 4-coordinate geometry to one C(24), one N(15), one H(41), and one H(42) atom. The C(23)-C(24) bond length is 1.41 Å. The C(23)-N(15) bond length is 1.50 Å. The C(23)-H(41) bond length is 0.96 Å. The C(23)-H(42) bond length is 0.96 Å. In the twenty-fourth C site, C(24) is bonded in a 3-coordinate geometry to one C(23), one O(1), and one O(2) atom. The C(24)-O(1) bond length is 1.33 Å. The C(24)-O(2) bond length is 1.25 Å. In the twenty-fifth C site, C(25) is bonded in a 3-coordinate geometry to one C(26), one N(16), one H(43), and one H(44) atom. The C(25)-C(26) bond length is 1.45 Å. The C(25)-N(16) bond length is 1.46 Å. The C(25)-H(43) bond length is 0.96 Å. The C(25)-H(44) bond length is 0.96 Å. In the twenty-sixth C site, C(26) is bonded in a bent 120 degrees geometry to one C(25) and one O(3) atom. The C(26)-O(3) bond length is 1.37 Å. In the twenty-seventh C site, C(27) is bonded in a distorted single-bond geometry to one C(28) and one N(17) atom. The C(27)-C(28) bond length is 1.55 Å. The C(27)-N(17) bond length is 1.46 Å. In the twenty-eighth C site, C(28) is bonded in an L-shaped geometry to one C(27) and one O(4) atom. The C(28)-O(4) bond length is 1.44 Å. In the twenty-ninth C site, C(29) is bonded in a distorted single-bond geometry to one N(18) atom. The C(29)-N(18) bond length is 1.47 Å. In the thirtieth C site, C(30) is bonded in a distorted single-bond geometry to one N(18) atom. The C(30)-N(18) bond length is 1.47 Å. There are eighteen inequivalent N sites. In the first N site, N(1) is bonded in a single-bond geometry to one C(2) atom. In the second N site, N(2) is bonded in a single-bond geometry to one C(4) atom. In the third N site, N(3) is bonded in a bent 150 degrees geometry to one Ni(2) and one C(5) atom. In the fourth N site, N(4) is bonded in a distorted bent 150 degrees geometry to one Ni(1) and one C(1) atom. In the fifth N site, N(5) is bonded in a bent 150 degrees geometry to one Ni(3) and one C(3) atom. In the sixth N site, N(6) is bonded in a bent 150 degrees geometry to one Ni(1) and one C(6) atom. In the seventh N site, N(7) is bonded in a distorted single-bond geometry to one Ni(2), one C(10), one C(8), and one H(1) atom. The N(7)-H(1) bond length is 0.90 Å. In the eighth N site, N(8) is bonded in a distorted single-bond geometry to one Ni(2), one C(7), one C(9), and one H(2) atom. The N(8)-H(2) bond length is 0.90 Å. In the ninth N site, N(9) is bonded in a 1-coordinate geometry to one Ni(1), one C(15), one C(16), and one H(3) atom. The N(9)-H(3) bond length is 0.90 Å. In the tenth N site, N(10) is bonded in a distorted single-bond geometry to one Ni(1), one C(11), and one H(4) atom. The N(10)-H(4) bond length is 0.90 Å. In the eleventh N site, N(11) is bonded in a 1-coordinate geometry to one Ni(1), one C(18), and one H(5) atom. The N(11)-H(5) bond length is 0.90 Å. In the twelfth N site, N(12) is bonded in a 4-coordinate geometry to one Ni(1), one C(13), one C(14), and one H(6) atom. The N(12)-H(6) bond length is 0.90 Å. In the thirteenth N site, N(13) is bonded in a 1-coordinate geometry to one Ni(3), one C(19), one C(22), and one H(31) atom. The N(13)-H(31) bond length is 0.90 Å. In the fourteenth N site, N(14) is bonded in a distorted single-bond geometry to one Ni(3), one C(20), one C(21), and one H(34) atom. The N(14)-H(34) bond length is 0.90 Å. In the fifteenth N site, N(15) is bonded in a trigonal non-coplanar geometry to one C(21), one C(22), and one C(23) atom. In the sixteenth N site, N(16) is bonded in a trigonal non-coplanar geometry to one C(10), one C(25), and one C(9) atom. In the seventeenth N site, N(17) is bonded in a trigonal planar geometry to one C(11), one C(18), and one C(27) atom. In the eighteenth N site, N(18) is bonded in a distorted tetrahedral geometry to one C(14), one C(15), one C(29), and one C(30) atom. There are forty-four inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one N(7) atom. In the second H site, H(2) is bonded in a single-bond geometry to one N(8) atom. In the third H site, H(3) is bonded in a single-bond geometry to one N(9) atom. In the fourth H site, H(4) is bonded in a single-bond geometry to one N(10) atom. In the fifth H site, H(5) is bonded in a single-bond geometry to one N(11) atom. In the sixth H site, H(6) is bonded in a single-bond geometry to one N(12) atom. In the seventh H site, H(7) is bonded in a single-bond geometry to one C(7) atom. In the eighth H site, H(8) is bonded in a single-bond geometry to one C(7) atom. In the ninth H site, H(9) is bonded in a single-bond geometry to one C(8) atom. In the tenth H site, H(10) is bonded in a single-bond geometry to one C(8) atom. In the eleventh H site, H(11) is bonded in a single-bond geometry to one C(9) atom. In the twelfth H site, H(12) is bonded in a single-bond geometry to one C(9) atom. In the thirteenth H site, H(13) is bonded in a single-bond geometry to one C(10) atom. In the fourteenth H site, H(14) is bonded in a single-bond geometry to one C(10) atom. In the fifteenth H site, H(15) is bonded in a single-bond geometry to one C(11) atom. In the sixteenth H site, H(16) is bonded in a single-bond geometry to one C(11) atom. In the seventeenth H site, H(17) is bonded in a single-bond geometry to one C(12) atom. In the eighteenth H site, H(18) is bonded in a single-bond geometry to one C(12) atom. In the nineteenth H site, H(19) is bonded in a single-bond geometry to one C(13) atom. In the twentieth H site, H(20) is bonded in a single-bond geometry to one C(13) atom. In the twenty-first H site, H(21) is bonded in a single-bond geometry to one C(14) atom. In the twenty-second H site, H(22) is bonded in a single-bond geometry to one C(14) atom. In the twenty-third H site, H(23) is bonded in a single-bond geometry to one C(15) atom. In the twenty-fourth H site, H(24) is bonded in a single-bond geometry to one C(15) atom. In the twenty-fifth H site, H(25) is bonded in a single-bond geometry to one C(16) atom. In the twenty-sixth H site, H(26) is bonded in a single-bond geometry to one C(16) atom. In the twenty-seventh H site, H(27) is bonded in a single-bond geometry to one C(17) atom. In the twenty-eighth H site, H(28) is bonded in a single-bond geometry to one C(17) atom. In the twenty-ninth H site, H(29) is bonded in a single-bond geometry to one C(18) atom. In the thirtieth H site, H(30) is bonded in a single-bond geometry to one C(18) atom. In the thirty-first H site, H(31) is bonded in a single-bond geometry to one N(13) atom. In the thirty-second H site, H(32) is bonded in a single-bond geometry to one C(19) atom. In the thirty-third H site, H(33) is bonded in a single-bond geometry to one C(19) atom. In the thirty-fourth H site, H(34) is bonded in a single-bond geometry to one N(14) atom. In the thirty-fifth H site, H(35) is bonded in a single-bond geometry to one C(20) atom. In the thirty-sixth H site, H(36) is bonded in a single-bond geometry to one C(20) atom. In the thirty-seventh H site, H(37) is bonded in a single-bond geometry to one C(21) atom. In the thirty-eighth H site, H(38) is bonded in a single-bond geometry to one C(21) atom. In the thirty-ninth H site, H(39) is bonded in a single-bond geometry to one C(22) atom. In the fortieth H site, H(40) is bonded in a single-bond geometry to one C(22) atom. In the forty-first H site, H(41) is bonded in a single-bond geometry to one C(23) atom. In the forty-second H site, H(42) is bonded in a single-bond geometry to one C(23) atom. In the forty-third H site, H(43) is bonded in a single-bond geometry to one C(25) atom. In the forty-fourth H site, H(44) is bonded in a single-bond geometry to one C(25) atom. There are four inequivalent O sites. In the first O site, O(1) is bonded in a single-bond geometry to one C(24) atom. In the second O site, O(2) is bonded in a single-bond geometry to one C(24) atom. In the third O site, O(3) is bonded in a single-bond geometry to one C(26) atom. In the fourth O site, O(4) is bonded in a single-bond geometry to one C(28) atom. Linkers: 2 C1CNCN(C[C]2OO2)CNCCNCN(C[C]2OO2)CN1 ,2 [O][C]CN1CNCCNCN(C[C][O])CNCCNC1. Metal clusters: 8 [Fe] ,16 [Ni]. The MOF has largest included sphere 5.21 A, density 1.30 g/cm3, surface area 4650.36 m2/g, accessible volume 0.25 cm3/g