Li4Ni2P4H3O16 crystallizes in the triclinic P1 space group. There are four inequivalent Li sites. In the first Li site, Li(1) is bonded in a 5-coordinate geometry to one O(1), one O(13), one O(14), one O(4), and one O(6) atom. In the second Li site, Li(2) is bonded in a 5-coordinate geometry to one O(10), one O(15), one O(5), one O(7), and one O(9) atom. In the third Li site, Li(3) is bonded in a 5-coordinate geometry to one O(10), one O(12), one O(2), one O(7), and one O(8) atom. In the fourth Li site, Li(4) is bonded in a 5-coordinate geometry to one O(11), one O(13), one O(16), one O(3), and one O(4) atom. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(12), one O(14), one O(15), one O(2), one O(3), and one O(5) atom to form NiO6 octahedra that share  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(4)O4 tetrahedra, corners with two equivalent P(2)O4 tetrahedra, and corners with two equivalent P(3)O4 tetrahedra. In the second Ni site, Ni(2) is bonded to one O(1), one O(11), one O(16), one O(6), one O(8), and one O(9) atom to form NiO6 octahedra that share  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra, corners with two equivalent P(1)O4 tetrahedra, and corners with two equivalent P(4)O4 tetrahedra. There are four inequivalent P sites. In the first P site, P(1) is bonded to one O(16), one O(2), one O(4), and one O(8) atom to form PO4 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 30-53°. In the second P site, P(2) is bonded to one O(11), one O(12), one O(3), and one O(7) atom to form PO4 tetrahedra that share  a cornercorner with one Ni(2)O6 octahedra and corners with two equivalent Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 21-54°. In the third P site, P(3) is bonded to one O(10), one O(14), one O(5), and one O(6) atom to form PO4 tetrahedra that share  a cornercorner with one Ni(2)O6 octahedra and corners with two equivalent Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 23-55°. In the fourth P site, P(4) is bonded to one O(1), one O(13), one O(15), and one O(9) atom to form PO4 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 30-53°. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(4) atom. In the second H site, H(2) is bonded in a single-bond geometry to one O(13) atom. In the third H site, H(3) is bonded in a linear geometry to one O(10) and one O(7) atom. There are sixteen inequivalent O sites. In the first O site, O(1) is bonded in a distorted T-shaped geometry to one Li(1), one Ni(2), and one P(4) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to one Li(3), one Ni(1), and one P(1) atom. In the third O site, O(3) is bonded in a trigonal planar geometry to one Li(4), one Ni(1), and one P(2) atom. In the fourth O site, O(4) is bonded in a 1-coordinate geometry to one Li(1), one Li(4), one P(1), and one H(1) atom. In the fifth O site, O(5) is bonded in a distorted T-shaped geometry to one Li(2), one Ni(1), and one P(3) atom. In the sixth O site, O(6) is bonded in a 3-coordinate geometry to one Li(1), one Ni(2), and one P(3) atom. In the seventh O site, O(7) is bonded in a 4-coordinate geometry to one Li(2), one Li(3), one P(2), and one H(3) atom. In the eighth O site, O(8) is bonded in a distorted trigonal planar geometry to one Li(3), one Ni(2), and one P(1) atom. In the ninth O site, O(9) is bonded in a distorted trigonal planar geometry to one Li(2), one Ni(2), and one P(4) atom. In the tenth O site, O(10) is bonded in a 4-coordinate geometry to one Li(2), one Li(3), one P(3), and one H(3) atom. In the eleventh O site, O(11) is bonded in a distorted trigonal non-coplanar geometry to one Li(4), one Ni(2), and one P(2) atom. In the twelfth O site, O(12) is bonded in a distorted T-shaped geometry to one Li(3), one Ni(1), and one P(2) atom. In the thirteenth O site, O(13) is bonded in a 1-coordinate geometry to one Li(1), one Li(4), one P(4), and one H(2) atom. In the fourteenth O site, O(14) is bonded in a trigonal planar geometry to one Li(1), one Ni(1), and one P(3) atom. In the fifteenth O site, O(15) is bonded in a distorted trigonal non-coplanar geometry to one Li(2), one Ni(1), and one P(4) atom. In the sixteenth O site, O(16) is bonded in a distorted T-shaped geometry to one Li(4), one Ni(2), and one P(1) atom.
Li4Ni2P4H3O16 crystallizes in the triclinic P1 space group. There are four inequivalent Li sites. In the first Li site, Li(1) is bonded in a 5-coordinate geometry to one O(1), one O(13), one O(14), one O(4), and one O(6) atom. The Li(1)-O(1) bond length is 2.01 Å. The Li(1)-O(13) bond length is 2.52 Å. The Li(1)-O(14) bond length is 1.99 Å. The Li(1)-O(4) bond length is 2.09 Å. The Li(1)-O(6) bond length is 1.99 Å. In the second Li site, Li(2) is bonded in a 5-coordinate geometry to one O(10), one O(15), one O(5), one O(7), and one O(9) atom. The Li(2)-O(10) bond length is 2.47 Å. The Li(2)-O(15) bond length is 2.00 Å. The Li(2)-O(5) bond length is 1.98 Å. The Li(2)-O(7) bond length is 1.98 Å. The Li(2)-O(9) bond length is 1.97 Å. In the third Li site, Li(3) is bonded in a 5-coordinate geometry to one O(10), one O(12), one O(2), one O(7), and one O(8) atom. The Li(3)-O(10) bond length is 2.03 Å. The Li(3)-O(12) bond length is 1.97 Å. The Li(3)-O(2) bond length is 2.02 Å. The Li(3)-O(7) bond length is 2.42 Å. The Li(3)-O(8) bond length is 1.95 Å. In the fourth Li site, Li(4) is bonded in a 5-coordinate geometry to one O(11), one O(13), one O(16), one O(3), and one O(4) atom. The Li(4)-O(11) bond length is 1.99 Å. The Li(4)-O(13) bond length is 2.10 Å. The Li(4)-O(16) bond length is 2.02 Å. The Li(4)-O(3) bond length is 2.00 Å. The Li(4)-O(4) bond length is 2.53 Å. There are two inequivalent Ni sites. In the first Ni site, Ni(1) is bonded to one O(12), one O(14), one O(15), one O(2), one O(3), and one O(5) atom to form NiO6 octahedra that share  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(4)O4 tetrahedra, corners with two equivalent P(2)O4 tetrahedra, and corners with two equivalent P(3)O4 tetrahedra. The Ni(1)-O(12) bond length is 2.12 Å. The Ni(1)-O(14) bond length is 2.07 Å. The Ni(1)-O(15) bond length is 2.03 Å. The Ni(1)-O(2) bond length is 2.02 Å. The Ni(1)-O(3) bond length is 2.01 Å. The Ni(1)-O(5) bond length is 2.17 Å. In the second Ni site, Ni(2) is bonded to one O(1), one O(11), one O(16), one O(6), one O(8), and one O(9) atom to form NiO6 octahedra that share  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra, corners with two equivalent P(1)O4 tetrahedra, and corners with two equivalent P(4)O4 tetrahedra. The Ni(2)-O(1) bond length is 2.02 Å. The Ni(2)-O(11) bond length is 2.13 Å. The Ni(2)-O(16) bond length is 2.02 Å. The Ni(2)-O(6) bond length is 2.16 Å. The Ni(2)-O(8) bond length is 2.12 Å. The Ni(2)-O(9) bond length is 2.12 Å. There are four inequivalent P sites. In the first P site, P(1) is bonded to one O(16), one O(2), one O(4), and one O(8) atom to form PO4 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 30-53°. The P(1)-O(16) bond length is 1.51 Å. The P(1)-O(2) bond length is 1.53 Å. The P(1)-O(4) bond length is 1.64 Å. The P(1)-O(8) bond length is 1.53 Å. In the second P site, P(2) is bonded to one O(11), one O(12), one O(3), and one O(7) atom to form PO4 tetrahedra that share  a cornercorner with one Ni(2)O6 octahedra and corners with two equivalent Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 21-54°. The P(2)-O(11) bond length is 1.55 Å. The P(2)-O(12) bond length is 1.54 Å. The P(2)-O(3) bond length is 1.58 Å. The P(2)-O(7) bond length is 1.54 Å. In the third P site, P(3) is bonded to one O(10), one O(14), one O(5), and one O(6) atom to form PO4 tetrahedra that share  a cornercorner with one Ni(2)O6 octahedra and corners with two equivalent Ni(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 23-55°. The P(3)-O(10) bond length is 1.60 Å. The P(3)-O(14) bond length is 1.55 Å. The P(3)-O(5) bond length is 1.52 Å. The P(3)-O(6) bond length is 1.53 Å. In the fourth P site, P(4) is bonded to one O(1), one O(13), one O(15), and one O(9) atom to form PO4 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 30-53°. The P(4)-O(1) bond length is 1.52 Å. The P(4)-O(13) bond length is 1.64 Å. The P(4)-O(15) bond length is 1.53 Å. The P(4)-O(9) bond length is 1.53 Å. There are three inequivalent H sites. In the first H site, H(1) is bonded in a single-bond geometry to one O(4) atom. The H(1)-O(4) bond length is 0.98 Å. In the second H site, H(2) is bonded in a single-bond geometry to one O(13) atom. The H(2)-O(13) bond length is 0.97 Å. In the third H site, H(3) is bonded in a linear geometry to one O(10) and one O(7) atom. The H(3)-O(10) bond length is 1.03 Å. The H(3)-O(7) bond length is 1.58 Å. There are sixteen inequivalent O sites. In the first O site, O(1) is bonded in a distorted T-shaped geometry to one Li(1), one Ni(2), and one P(4) atom. In the second O site, O(2) is bonded in a 3-coordinate geometry to one Li(3), one Ni(1), and one P(1) atom. In the third O site, O(3) is bonded in a trigonal planar geometry to one Li(4), one Ni(1), and one P(2) atom. In the fourth O site, O(4) is bonded in a 1-coordinate geometry to one Li(1), one Li(4), one P(1), and one H(1) atom. In the fifth O site, O(5) is bonded in a distorted T-shaped geometry to one Li(2), one Ni(1), and one P(3) atom. In the sixth O site, O(6) is bonded in a 3-coordinate geometry to one Li(1), one Ni(2), and one P(3) atom. In the seventh O site, O(7) is bonded in a 4-coordinate geometry to one Li(2), one Li(3), one P(2), and one H(3) atom. In the eighth O site, O(8) is bonded in a distorted trigonal planar geometry to one Li(3), one Ni(2), and one P(1) atom. In the ninth O site, O(9) is bonded in a distorted trigonal planar geometry to one Li(2), one Ni(2), and one P(4) atom. In the tenth O site, O(10) is bonded in a 4-coordinate geometry to one Li(2), one Li(3), one P(3), and one H(3) atom. In the eleventh O site, O(11) is bonded in a distorted trigonal non-coplanar geometry to one Li(4), one Ni(2), and one P(2) atom. In the twelfth O site, O(12) is bonded in a distorted T-shaped geometry to one Li(3), one Ni(1), and one P(2) atom. In the thirteenth O site, O(13) is bonded in a 1-coordinate geometry to one Li(1), one Li(4), one P(4), and one H(2) atom. In the fourteenth O site, O(14) is bonded in a trigonal planar geometry to one Li(1), one Ni(1), and one P(3) atom. In the fifteenth O site, O(15) is bonded in a distorted trigonal non-coplanar geometry to one Li(2), one Ni(1), and one P(4) atom. In the sixteenth O site, O(16) is bonded in a distorted T-shaped geometry to one Li(4), one Ni(2), and one P(1) atom.