Ni3H20(C11O7)2 crystallizes in the triclinic P1 space group. There are five inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(2); one O(4); two equivalent O(13,15); and two equivalent O(25,27) atoms to form corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles range from 61-62°. The Ni(1)-O(2) bond length is 2.05 Å. The Ni(1)-O(4) bond length is 2.05 Å. Both Ni(1)-O(13,15) bond lengths are 2.04 Å. Both Ni(1)-O(25,27) bond lengths are 2.03 Å. In the second Ni site, Ni(2) is bonded to one O(1), one O(14), one O(16), one O(26), one O(28), and one O(3) atom to form corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles range from 60-63°. The Ni(2)-O(1) bond length is 2.05 Å. The Ni(2)-O(14) bond length is 2.05 Å. The Ni(2)-O(16) bond length is 2.03 Å. The Ni(2)-O(26) bond length is 2.03 Å. The Ni(2)-O(28) bond length is 2.03 Å. The Ni(2)-O(3) bond length is 2.04 Å. In the third Ni site, Ni(3,5) is bonded to one O(17,19); one O(21); one O(6,8); one O(9,11); and two equivalent O(25,27) atoms to form a mixture of edge and corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles range from 61-62°. The Ni(3,5)-O(17,19) bond length is 2.15 Å. The Ni(3,5)-O(21) bond length is 2.10 Å. The Ni(3,5)-O(6,8) bond length is 2.08 Å. The Ni(3,5)-O(9,11) bond length is 2.18 Å. Both Ni(3,5)-O(25,27) bond lengths are 2.04 Å. In the fourth Ni site, Ni(4) is bonded to one O(10), one O(18), one O(22), one O(26), one O(28), and one O(5) atom to form a mixture of edge and corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles range from 60-61°. The Ni(4)-O(10) bond length is 2.19 Å. The Ni(4)-O(18) bond length is 2.14 Å. The Ni(4)-O(22) bond length is 2.09 Å. The Ni(4)-O(26) bond length is 2.03 Å. The Ni(4)-O(28) bond length is 2.04 Å. The Ni(4)-O(5) bond length is 2.08 Å. In the fifth Ni site, Ni(6) is bonded to one O(12), one O(20), one O(24), one O(26), one O(28), and one O(7) atom to form a mixture of edge and corner-sharing NiO6 octahedra. The corner-sharing octahedral tilt angles range from 62-63°. The Ni(6)-O(12) bond length is 2.18 Å. The Ni(6)-O(20) bond length is 2.14 Å. The Ni(6)-O(24) bond length is 2.09 Å. The Ni(6)-O(26) bond length is 2.05 Å. The Ni(6)-O(28) bond length is 2.04 Å. The Ni(6)-O(7) bond length is 2.08 Å. There are thirty inequivalent C sites. In the first C site, C(1) is bonded in a distorted bent 120 degrees geometry to one C(5), one O(1), and one O(5) atom. The C(1)-C(5) bond length is 1.50 Å. The C(1)-O(1) bond length is 1.28 Å. The C(1)-O(5) bond length is 1.27 Å. In the second C site, C(2,4) is bonded in a distorted bent 120 degrees geometry to one C(6); one O(2); and one O(6,8) atom. The C(2,4)-C(6) bond length is 1.50 Å. The C(2,4)-O(2) bond length is 1.28 Å. The C(2,4)-O(6,8) bond length is 1.27 Å. In the third C site, C(3) is bonded in a distorted bent 120 degrees geometry to one C(7), one O(3), and one O(7) atom. The C(3)-C(7) bond length is 1.50 Å. The C(3)-O(3) bond length is 1.28 Å. The C(3)-O(7) bond length is 1.27 Å. In the fourth C site, C(5) is bonded in a trigonal planar geometry to one C(1), one C(25), and one C(9) atom. The C(5)-C(25) bond length is 1.40 Å. The C(5)-C(9) bond length is 1.41 Å. In the fifth C site, C(6) is bonded in a trigonal planar geometry to one C(10); one C(2,4); and one C(26) atom. The C(6)-C(10) bond length is 1.41 Å. The C(6)-C(26) bond length is 1.40 Å. In the sixth C site, C(7) is bonded in a trigonal planar geometry to one C(11,12); one C(27,28); and one C(3) atom. The C(7)-C(11,12) bond length is 1.41 Å. The C(7)-C(27,28) bond length is 1.40 Å. In the seventh C site, C(8) is bonded in a trigonal planar geometry to one C(11,12); one C(2,4); and one C(27,28) atom. The C(8)-C(11,12) bond length is 1.41 Å. The C(8)-C(2,4) bond length is 1.50 Å. The C(8)-C(27,28) bond length is 1.40 Å. In the eighth C site, C(9) is bonded in a distorted single-bond geometry to one C(13,15,16); one C(5); and one H(1,3,4) atom. The C(9)-C(13,15,16) bond length is 1.40 Å. The C(9)-H(1,3,4) bond length is 1.09 Å. In the ninth C site, C(10) is bonded in a distorted single-bond geometry to one C(14), one C(6), and one H(2) atom. The C(10)-C(14) bond length is 1.40 Å. The C(10)-H(2) bond length is 1.09 Å. In the tenth C site, C(11,12) is bonded in a distorted single-bond geometry to one C(13,15,16); one C(7); and one H(1,3,4) atom. The C(11,12)-C(13,15,16) bond length is 1.40 Å. The C(11,12)-H(1,3,4) bond length is 1.09 Å. In the eleventh C site, C(13,15,16) is bonded in a distorted trigonal planar geometry to one C(17,19,20); one C(9); and one H(5,7,8) atom. The C(13,15,16)-C(17,19,20) bond length is 1.40 Å. The C(13,15,16)-H(5,7,8) bond length is 1.09 Å. In the twelfth C site, C(14) is bonded in a distorted trigonal planar geometry to one C(10), one C(18), and one H(6) atom. The C(14)-C(18) bond length is 1.40 Å. The C(14)-H(6) bond length is 1.09 Å. In the thirteenth C site, C(17,19,20) is bonded in a distorted trigonal planar geometry to one C(13,15,16); one C(21,23,24); and one H(9,11,12) atom. The C(17,19,20)-C(21,23,24) bond length is 1.40 Å. The C(17,19,20)-H(9,11,12) bond length is 1.09 Å. In the fourteenth C site, C(18) is bonded in a distorted trigonal planar geometry to one C(14), one C(22), and one H(10) atom. The C(18)-C(22) bond length is 1.40 Å. The C(18)-H(10) bond length is 1.09 Å. In the fifteenth C site, C(21,23,24) is bonded in a trigonal planar geometry to one C(17,19,20); one C(25); and one C(33,35) atom. The C(21,23,24)-C(25) bond length is 1.40 Å. The C(21,23,24)-C(33,35) bond length is 1.48 Å. In the sixteenth C site, C(22) is bonded in a trigonal planar geometry to one C(18), one C(26), and one C(34) atom. The C(22)-C(26) bond length is 1.40 Å. The C(22)-C(34) bond length is 1.48 Å. In the seventeenth C site, C(25) is bonded in a distorted trigonal planar geometry to one C(21,23,24); one C(5); and one H(13,14,15,16) atom. The C(25)-H(13,14,15,16) bond length is 1.09 Å. In the eighteenth C site, C(26) is bonded in a distorted trigonal planar geometry to one C(22); one C(6); and one H(13,14,15,16) atom. The C(26)-H(13,14,15,16) bond length is 1.09 Å. In the nineteenth C site, C(27,28) is bonded in a distorted trigonal planar geometry to one C(21,23,24); one C(7); and one H(13,14,15,16) atom. The C(27,28)-C(21,23,24) bond length is 1.40 Å. The C(27,28)-H(13,14,15,16) bond length is 1.09 Å. In the twentieth C site, C(29,31,32) is bonded in a distorted single-bond geometry to one C(33,35); one C(37,39); and one H(17,18,19) atom. The C(29,31,32)-C(33,35) bond length is 1.40 Å. The C(29,31,32)-C(37,39) bond length is 1.40 Å. The C(29,31,32)-H(17,18,19) bond length is 1.09 Å. In the twenty-first C site, C(30) is bonded in a distorted single-bond geometry to one C(34); one C(40); and one H(17,18,19) atom. The C(30)-C(34) bond length is 1.40 Å. The C(30)-C(40) bond length is 1.40 Å. The C(30)-H(17,18,19) bond length is 1.09 Å. In the twenty-second C site, C(33,35) is bonded in a trigonal planar geometry to one C(21,23,24); one C(29,31,32); and one C(37,39) atom. The C(33,35)-C(37,39) bond length is 1.41 Å. In the twenty-third C site, C(34) is bonded in a trigonal planar geometry to one C(22), one C(30), and one C(38) atom. The C(34)-C(38) bond length is 1.41 Å. In the twenty-fourth C site, C(36) is bonded in a trigonal planar geometry to one C(21,23,24); one C(29,31,32); and one C(40) atom. The C(36)-C(21,23,24) bond length is 1.48 Å. The C(36)-C(29,31,32) bond length is 1.40 Å. The C(36)-C(40) bond length is 1.41 Å. In the twenty-fifth C site, C(37,39) is bonded in a trigonal planar geometry to one C(29,31,32); one C(33,35); and one C(41,43) atom. The C(37,39)-C(41,43) bond length is 1.51 Å. In the twenty-sixth C site, C(38) is bonded in a trigonal planar geometry to one C(29,31,32); one C(34); and one C(42) atom. The C(38)-C(29,31,32) bond length is 1.40 Å. The C(38)-C(42) bond length is 1.51 Å. In the twenty-seventh C site, C(40) is bonded in a trigonal planar geometry to one C(30), one C(36), and one C(44) atom. The C(40)-C(44) bond length is 1.51 Å. In the twenty-eighth C site, C(41,43) is bonded in a distorted bent 120 degrees geometry to one C(37,39); one O(13,15); and one O(9,11) atom. The C(41,43)-O(13,15) bond length is 1.28 Å. The C(41,43)-O(9,11) bond length is 1.26 Å. In the twenty-ninth C site, C(42) is bonded in a distorted bent 120 degrees geometry to one C(38), one O(10), and one O(14) atom. The C(42)-O(10) bond length is 1.26 Å. The C(42)-O(14) bond length is 1.28 Å. In the thirtieth C site, C(44) is bonded in a distorted bent 120 degrees geometry to one C(40), one O(12), and one O(16) atom. The C(44)-O(12) bond length is 1.26 Å. The C(44)-O(16) bond length is 1.28 Å. There are twenty-four inequivalent H sites. In the first H site, H(1,3,4) is bonded in a single-bond geometry to one C(9) atom. In the second H site, H(2) is bonded in a single-bond geometry to one C(10) atom. In the third H site, H(5,7,8) is bonded in a single-bond geometry to one C(13,15,16) atom. In the fourth H site, H(6) is bonded in a single-bond geometry to one C(14) atom. In the fifth H site, H(9,11,12) is bonded in a single-bond geometry to one C(17,19,20) atom. In the sixth H site, H(10) is bonded in a single-bond geometry to one C(18) atom. In the seventh H site, H(13,14,15,16) is bonded in a single-bond geometry to one C(25) atom. In the eighth H site, H(17,18,19) is bonded in a single-bond geometry to one C(29,31,32) atom. In the ninth H site, H(20) is bonded in a single-bond geometry to one C(29,31,32) atom. The H(20)-C(29,31,32) bond length is 1.09 Å. In the tenth H site, H(21,23) is bonded in a distorted linear geometry to one O(13,15) and one O(17,19) atom. The H(21,23)-O(13,15) bond length is 1.60 Å. The H(21,23)-O(17,19) bond length is 1.01 Å. In the eleventh H site, H(22) is bonded in a distorted linear geometry to one O(14) and one O(18) atom. The H(22)-O(14) bond length is 1.60 Å. The H(22)-O(18) bond length is 1.01 Å. In the twelfth H site, H(24) is bonded in a distorted linear geometry to one O(16) and one O(20) atom. The H(24)-O(16) bond length is 1.60 Å. The H(24)-O(20) bond length is 1.01 Å. In the thirteenth H site, H(25,27) is bonded in a single-bond geometry to one O(17,19) atom. The H(25,27)-O(17,19) bond length is 0.98 Å. In the fourteenth H site, H(26) is bonded in a single-bond geometry to one O(18) atom. The H(26)-O(18) bond length is 0.98 Å. In the fifteenth H site, H(28) is bonded in a single-bond geometry to one O(20) atom. The H(28)-O(20) bond length is 0.98 Å. In the sixteenth H site, H(29,31) is bonded in a single-bond geometry to one O(21) atom. The H(29,31)-O(21) bond length is 0.98 Å. In the seventeenth H site, H(30) is bonded in a single-bond geometry to one O(22) atom. The H(30)-O(22) bond length is 0.98 Å. In the eighteenth H site, H(32) is bonded in a single-bond geometry to one O(24) atom. The H(32)-O(24) bond length is 0.98 Å. In the nineteenth H site, H(33,35) is bonded in a distorted single-bond geometry to one O(2) and one O(21) atom. The H(33,35)-O(2) bond length is 1.67 Å. The H(33,35)-O(21) bond length is 1.00 Å. In the twentieth H site, H(34) is bonded in a distorted single-bond geometry to one O(1) and one O(22) atom. The H(34)-O(1) bond length is 1.68 Å. The H(34)-O(22) bond length is 1.00 Å. In the twenty-first H site, H(36) is bonded in a distorted single-bond geometry to one O(24) and one O(3) atom. The H(36)-O(24) bond length is 1.00 Å. The H(36)-O(3) bond length is 1.67 Å. In the twenty-second H site, H(37,39) is bonded in a single-bond geometry to one O(25,27) atom. The H(37,39)-O(25,27) bond length is 0.97 Å. In the twenty-third H site, H(38) is bonded in a single-bond geometry to one O(26) atom. The H(38)-O(26) bond length is 0.98 Å. In the twenty-fourth H site, H(40) is bonded in a single-bond geometry to one O(28) atom. The H(40)-O(28) bond length is 0.98 Å. There are twenty-three inequivalent O sites. In the first O site, O(1) is bonded in a distorted trigonal planar geometry to one Ni(2), one C(1), and one H(34) atom. In the second O site, O(2) is bonded in a distorted trigonal planar geometry to one Ni(1); one C(2,4); and one H(33,35) atom. In the third O site, O(3) is bonded in a distorted trigonal planar geometry to one Ni(2), one C(3), and one H(36) atom. In the fourth O site, O(4) is bonded in a distorted trigonal planar geometry to one Ni(1); one C(2,4); and one H(33,35) atom. The O(4)-C(2,4) bond length is 1.28 Å. The O(4)-H(33,35) bond length is 1.67 Å. In the fifth O site, O(5) is bonded in a bent 120 degrees geometry to one Ni(4) and one C(1) atom. In the sixth O site, O(6,8) is bonded in a bent 120 degrees geometry to one Ni(3,5) and one C(2,4) atom. In the seventh O site, O(7) is bonded in a bent 120 degrees geometry to one Ni(6) and one C(3) atom. In the eighth O site, O(9,11) is bonded in a bent 120 degrees geometry to one Ni(3,5) and one C(41,43) atom. In the ninth O site, O(10) is bonded in a bent 120 degrees geometry to one Ni(4) and one C(42) atom. In the tenth O site, O(12) is bonded in a bent 120 degrees geometry to one Ni(6) and one C(44) atom. In the eleventh O site, O(13,15) is bonded in a distorted trigonal planar geometry to one Ni(1); one C(41,43); and one H(21,23) atom. In the twelfth O site, O(14) is bonded in a distorted trigonal planar geometry to one Ni(2), one C(42), and one H(22) atom. In the thirteenth O site, O(16) is bonded in a distorted trigonal planar geometry to one Ni(2), one C(44), and one H(24) atom. In the fourteenth O site, O(17,19) is bonded in a distorted water-like geometry to one Ni(3,5); one H(21,23); and one H(25,27) atom. In the fifteenth O site, O(18) is bonded in a distorted water-like geometry to one Ni(4), one H(22), and one H(26) atom. In the sixteenth O site, O(20) is bonded in a distorted water-like geometry to one Ni(6), one H(24), and one H(28) atom. In the seventeenth O site, O(21) is bonded in a distorted water-like geometry to one Ni(3,5); one H(29,31); and one H(33,35) atom. In the eighteenth O site, O(22) is bonded in a distorted water-like geometry to one Ni(4), one H(30), and one H(34) atom. In the nineteenth O site, O(23) is bonded in a distorted water-like geometry to one Ni(3,5); one H(29,31); and one H(33,35) atom. The O(23)-Ni(3,5) bond length is 2.10 Å. The O(23)-H(29,31) bond length is 0.98 Å. The O(23)-H(33,35) bond length is 1.00 Å. In the twentieth O site, O(24) is bonded in a distorted water-like geometry to one Ni(6), one H(32), and one H(36) atom. In the twenty-first O site, O(25,27) is bonded in a distorted single-bond geometry to one Ni(1); two equivalent Ni(3,5); and one H(37,39) atom. In the twenty-second O site, O(26) is bonded in a distorted single-bond geometry to one Ni(2), one Ni(4), one Ni(6), and one H(38) atom. In the twenty-third O site, O(28) is bonded in a distorted single-bond geometry to one Ni(2), one Ni(4), one Ni(6), and one H(40) atom. Linkers: 2 [O]C(=O)c1cccc(-c2cc(C([O])=O)c(-c3cccc(C([O])=O)c3)cc2C([O])=O)c1 ,2 [O]C(=O)/[C]=C/[C]c1cc(C([O])=O)c(-c2cccc(C([O])=O)c2)cc1C([O])=O. Metal clusters: 6 [Ni]. The MOF has largest included sphere 1.54 A, density 2.06 g/cm3, surface area 3403.61 m2/g, accessible volume 0.07 cm3/g