Ni4C60N12H15(OF24)3 crystallizes in the cubic Fm-3m space group. Ni(1) is bonded to three equivalent N(1) and three equivalent O(1) atoms to form a mixture of distorted edge and corner-sharing NiN3O3 octahedra. The corner-sharing octahedral tilt angles are 12°. All Ni(1)-N(1) bond lengths are 1.97 Å. All Ni(1)-O(1) bond lengths are 1.88 Å. There are seven inequivalent C sites. In the first C site, C(5) is bonded in a trigonal planar geometry to one C(1), one C(5), and one C(6) atom. The C(5)-C(1) bond length is 1.39 Å. The C(5)-C(5) bond length is 1.39 Å. The C(5)-C(6) bond length is 1.54 Å. In the second C site, C(6) is bonded in a 6-coordinate geometry to one C(5), two equivalent F(1), two equivalent F(2), and two equivalent F(3) atoms. Both C(6)-F(1) bond lengths are 1.35 Å. Both C(6)-F(2) bond lengths are 1.35 Å. Both C(6)-F(3) bond lengths are 1.35 Å. In the third C site, C(7) is bonded in a distorted bent 120 degrees geometry to one C(4), one N(1), and one H(2) atom. The C(7)-C(4) bond length is 1.36 Å. The C(7)-N(1) bond length is 1.36 Å. The C(7)-H(2) bond length is 0.95 Å. In the fourth C site, C(1) is bonded in a trigonal planar geometry to one C(2) and two equivalent C(5) atoms. The C(1)-C(2) bond length is 1.50 Å. In the fifth C site, C(2) is bonded in a linear geometry to one C(1) and one C(3) atom. The C(2)-C(3) bond length is 1.24 Å. In the sixth C site, C(3) is bonded in a distorted linear geometry to one C(2) and one C(4) atom. The C(3)-C(4) bond length is 1.50 Å. In the seventh C site, C(4) is bonded in a trigonal planar geometry to one C(3) and two equivalent C(7) atoms. N(1) is bonded in a 3-coordinate geometry to one Ni(1), one C(7), and one N(1) atom. The N(1)-N(1) bond length is 1.36 Å. There are two inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(1) atom. The H(1)-O(1) bond length is 0.95 Å. In the second H site, H(2) is bonded in a single-bond geometry to one C(7) atom. O(1) is bonded in a single-bond geometry to four equivalent Ni(1) and one H(1) atom. There are three inequivalent F sites. In the first F site, F(1) is bonded in a single-bond geometry to one C(6) atom. In the second F site, F(2) is bonded in a single-bond geometry to one C(6) atom. In the third F site, F(3) is bonded in a single-bond geometry to one C(6) atom. Linkers: 2 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C].[C]c1[c]c(C#CC2=CN=N[CH]2)[c][c]c1C#C[C]1C=NN=C1 ,2 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C].[C]c1[c]c(C#CC2=CN=N[CH]2)[c][c]c1C#CC1=CN=N[CH]1 ,1 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C]c1c([C])c(C#CC2=C[N]N=C2)c([C])c([C])c1C#C[C]1C=NN=C1 ,3 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C]c1c([C])c(C#CC2=C[N]N=C2)c([C])c([C])c1C#CC1=CN=N[CH]1 ,1 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C]c1[c]c(C#CC2=C[N]N=C2)[c]c([C])c1C#C[C]1C=NN=C1 ,1 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C].[C]c1[c]c(C#CC2=C[N]N=C2)[c][c]c1C#C[C]1C=NN=C1 ,4 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C]c1c(C#CC2=CN=N[CH]2)[c][c]c(C#CC2=C[N]N=C2)c1[C] ,3 C(#Cc1[c][c]c(C#CC2=C[N]N=C2)[c][c]1)C1=C[N]N=C1.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C].[C] ,3 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C].[C]c1[c]c(C#CC2=C[N]N=C2)[c][c]c1C#CC1=C[N]N=C1 ,1 C(#Cc1[c][c]c(C#C[C]2C=NN=C2)[c][c]1)[C]1C=NN=C1.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C].[C] ,1 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C].[C]c1[c]c(C#C[C]2C=NN=C2)[c][c]c1C#C[C]1C=NN=C1 ,1 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C]c1[c]c(C#CC2=C[N]N=C2)c([C])c([C])c1C#C[C]1C=NN=C1 ,1 FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.FF.[C].[C].[C]c1c(C#C[C]2C=NN=C2)[c][c]c(C#CC2=C[N]N=C2)c1[C]. Metal clusters: 4 O[Ni]12(O)(O)[N][N][Ni@]3(O)[N][N][Ni]4[N][N][Ni]5[N][N][Ni]([N][N]3)[N][N][Ni@](O)([N][N][Ni]([N][N]5)[N][N][Ni@](O)([N][N]4)[N][N]1)[N][N]2. The MOF has largest included sphere 18.49 A, density 1.00 g/cm3, surface area 2740.54 m2/g, accessible volume 0.76 cm3/g