Ni3P6H44(C12O11)2 crystallizes in the triclinic P-1 space group. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to two equivalent O(3), two equivalent O(6), and two equivalent O(9) atoms to form NiO6 octahedra that share corners with two equivalent Ni(2)O6 octahedra, corners with two equivalent P(2)CO3 tetrahedra, and corners with two equivalent P(3)CO3 tetrahedra. The corner-sharing octahedral tilt angles are 59°. Both Ni(1)-O(3) bond lengths are 2.09 Å. Both Ni(1)-O(6) bond lengths are 2.17 Å. Both Ni(1)-O(9) bond lengths are 2.06 Å. In the second Ni site, Ni(2) is bonded to one O(1), one O(3), one O(5), one O(8), and two equivalent O(10) atoms to form NiO6 octahedra that share  a cornercorner with one Ni(1)O6 octahedra,  a cornercorner with one P(1)CO3 tetrahedra,  a cornercorner with one P(2)CO3 tetrahedra, corners with two equivalent P(3)CO3 tetrahedra, and  an edgeedge with one Ni(2)O6 octahedra. The corner-sharing octahedral tilt angles are 59°. The Ni(2)-O(1) bond length is 2.08 Å. The Ni(2)-O(3) bond length is 2.21 Å. The Ni(2)-O(5) bond length is 2.04 Å. The Ni(2)-O(8) bond length is 2.09 Å. There is one shorter (2.07 Å) and one longer (2.16 Å) Ni(2)-O(10) bond length. There are twelve inequivalent C sites. In the first C site, C(1) is bonded in a trigonal planar geometry to one C(2), one C(6), and one C(7) atom. The C(1)-C(2) bond length is 1.41 Å. The C(1)-C(6) bond length is 1.41 Å. The C(1)-C(7) bond length is 1.51 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(8) atom. The C(2)-C(3) bond length is 1.41 Å. The C(2)-C(8) bond length is 1.51 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(9) atom. The C(3)-C(4) bond length is 1.41 Å. The C(3)-C(9) bond length is 1.51 Å. In the fourth C site, C(4) is bonded in a trigonal planar geometry to one C(10), one C(3), and one C(5) atom. The C(4)-C(10) bond length is 1.50 Å. The C(4)-C(5) bond length is 1.41 Å. In the fifth C site, C(5) is bonded in a trigonal planar geometry to one C(11), one C(4), and one C(6) atom. The C(5)-C(11) bond length is 1.51 Å. The C(5)-C(6) bond length is 1.41 Å. In the sixth C site, C(6) is bonded in a trigonal planar geometry to one C(1), one C(12), and one C(5) atom. The C(6)-C(12) bond length is 1.51 Å. In the seventh C site, C(7) is bonded in a distorted water-like geometry to one C(1), one P(1), one H(8), and one H(9) atom. The C(7)-P(1) bond length is 1.82 Å. The C(7)-H(8) bond length is 1.10 Å. The C(7)-H(9) bond length is 1.10 Å. In the eighth C site, C(8) is bonded in a distorted trigonal non-coplanar geometry to one C(2), one H(10), one H(11), and one H(12) atom. The C(8)-H(10) bond length is 1.09 Å. The C(8)-H(11) bond length is 1.10 Å. The C(8)-H(12) bond length is 1.09 Å. In the ninth C site, C(9) is bonded in a distorted water-like geometry to one C(3), one P(2), one H(13), and one H(14) atom. The C(9)-P(2) bond length is 1.83 Å. The C(9)-H(13) bond length is 1.10 Å. The C(9)-H(14) bond length is 1.09 Å. In the tenth C site, C(10) is bonded in a distorted trigonal non-coplanar geometry to one C(4), one H(15), one H(16), and one H(17) atom. The C(10)-H(15) bond length is 1.09 Å. The C(10)-H(16) bond length is 1.10 Å. The C(10)-H(17) bond length is 1.10 Å. In the eleventh C site, C(11) is bonded in a distorted water-like geometry to one C(5), one P(3), one H(18), and one H(19) atom. The C(11)-P(3) bond length is 1.82 Å. The C(11)-H(18) bond length is 1.10 Å. The C(11)-H(19) bond length is 1.09 Å. In the twelfth C site, C(12) is bonded in a distorted trigonal non-coplanar geometry to one C(6), one H(20), one H(21), and one H(22) atom. The C(12)-H(20) bond length is 1.10 Å. The C(12)-H(21) bond length is 1.10 Å. The C(12)-H(22) bond length is 1.10 Å. There are three inequivalent P sites. In the first P site, P(1) is bonded to one C(7), one O(2), one O(4), and one O(5) atom to form distorted PCO3 tetrahedra that share  a cornercorner with one Ni(2)O6 octahedra. The corner-sharing octahedral tilt angles are 40°. The P(1)-O(2) bond length is 1.53 Å. The P(1)-O(4) bond length is 1.59 Å. The P(1)-O(5) bond length is 1.54 Å. In the second P site, P(2) is bonded to one C(9), one O(6), one O(7), and one O(8) atom to form PCO3 tetrahedra that share  a cornercorner with one Ni(1)O6 octahedra and  a cornercorner with one Ni(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 40-51°. The P(2)-O(6) bond length is 1.53 Å. The P(2)-O(7) bond length is 1.57 Å. The P(2)-O(8) bond length is 1.54 Å. In the third P site, P(3) is bonded to one C(11), one O(10), one O(11), and one O(9) atom to form PCO3 tetrahedra that share  a cornercorner with one Ni(1)O6 octahedra and corners with two equivalent Ni(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 47-54°. The P(3)-O(10) bond length is 1.56 Å. The P(3)-O(11) bond length is 1.58 Å. The P(3)-O(9) bond length is 1.52 Å. There are twenty-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 0.98 Å. In the second H site, H(2) is bonded in a distorted linear geometry to one O(1) and one O(6) atom. The H(2)-O(1) bond length is 1.02 Å. The H(2)-O(6) bond length is 1.58 Å. In the third H site, H(3) is bonded in a single-bond geometry to one O(3) atom. The H(3)-O(3) bond length is 0.98 Å. In the fourth H site, H(4) is bonded in a distorted single-bond geometry to one O(3) and one O(8) atom. The H(4)-O(3) bond length is 1.02 Å. The H(4)-O(8) bond length is 1.63 Å. In the fifth H site, H(5) is bonded in a linear geometry to one O(2) and one O(4) atom. The H(5)-O(2) bond length is 1.53 Å. The H(5)-O(4) bond length is 1.04 Å. In the sixth H site, H(6) is bonded in a distorted single-bond geometry to one O(2) and one O(7) atom. The H(6)-O(2) bond length is 1.66 Å. The H(6)-O(7) bond length is 1.01 Å. In the seventh H site, H(7) is bonded in a distorted linear geometry to one O(11) and one O(5) atom. The H(7)-O(11) bond length is 1.01 Å. The H(7)-O(5) bond length is 1.60 Å. 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(7) 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(8) atom. In the twelfth H site, H(12) is bonded in a single-bond geometry to one C(8) atom. In the thirteenth H site, H(13) is bonded in a single-bond geometry to one C(9) atom. In the fourteenth H site, H(14) is bonded in a single-bond geometry to one C(9) atom. In the fifteenth H site, H(15) is bonded in a single-bond geometry to one C(10) atom. In the sixteenth H site, H(16) is bonded in a single-bond geometry to one C(10) atom. In the seventeenth H site, H(17) is bonded in a single-bond geometry to one C(10) atom. In the eighteenth H site, H(18) is bonded in a single-bond geometry to one C(11) atom. In the nineteenth H site, H(19) is bonded in a single-bond geometry to one C(11) atom. In the twentieth H site, H(20) is bonded in a single-bond geometry to one C(12) atom. In the twenty-first H site, H(21) is bonded in a single-bond geometry to one C(12) atom. In the twenty-second H site, H(22) is bonded in a single-bond geometry to one C(12) atom. There are eleven inequivalent O sites. In the first O site, O(1) is bonded in a distorted water-like geometry to one Ni(2), one H(1), and one H(2) atom. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to one P(1), one H(5), and one H(6) atom. In the third O site, O(3) is bonded in a distorted water-like geometry to one Ni(1), one Ni(2), one H(3), and one H(4) atom. In the fourth O site, O(4) is bonded in a bent 120 degrees geometry to one P(1) and one H(5) atom. In the fifth O site, O(5) is bonded in a distorted trigonal non-coplanar geometry to one Ni(2), one P(1), and one H(7) atom. In the sixth O site, O(6) is bonded in a distorted trigonal planar geometry to one Ni(1), one P(2), and one H(2) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one P(2) and one H(6) atom. In the eighth O site, O(8) is bonded in a distorted trigonal non-coplanar geometry to one Ni(2), one P(2), and one H(4) atom. In the ninth O site, O(9) is bonded in a distorted bent 120 degrees geometry to one Ni(1) and one P(3) atom. In the tenth O site, O(10) is bonded in a distorted trigonal planar geometry to two equivalent Ni(2) and one P(3) atom. In the eleventh O site, O(11) is bonded in a water-like geometry to one P(3) and one H(7) atom. Linkers: 2 Cc1c(CP([O])(=O)O)c(C)c(CP([O])(=O)O)c(C)c1CP([O])(=O)O. Metal clusters: 3 [Ni]. The MOF has largest included sphere 2.55 A, density 1.89 g/cm3, surface area 3332.25 m2/g, accessible volume 0.08 cm3/g