KLiSb(PO4)2 crystallizes in the triclinic P1 space group. There are three inequivalent K sites. In the first K site, K(1) is bonded in a 9-coordinate geometry to one O(16), one O(23), one O(3), one O(6), one O(7), two equivalent O(17), and two equivalent O(18) atoms. In the second K site, K(2) is bonded in a 8-coordinate geometry to one O(1), one O(13), one O(19), one O(21), one O(24), one O(8), and two equivalent O(6) atoms. In the third K site, K(3) is bonded in a 4-coordinate geometry to one O(18), one O(19), one O(7), and one O(8) atom. There are three inequivalent Li sites. In the first Li site, Li(1) is bonded in a rectangular see-saw-like geometry to one O(1), one O(11), one O(21), and one O(6) atom. In the second Li site, Li(2) is bonded in a distorted rectangular see-saw-like geometry to one O(14), one O(19), one O(24), and one O(4) atom. In the third Li site, Li(3) is bonded in a 5-coordinate geometry to one O(10), one O(17), one O(18), one O(20), and one O(22) atom. There are three inequivalent Sb sites. In the first Sb site, Sb(1) is bonded to one O(12), one O(15), one O(2), one O(3), one O(5), and one O(9) atom to form SbO6 octahedra that share  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra, corners with two equivalent P(5)O4 tetrahedra, and corners with two equivalent P(6)O4 tetrahedra. In the second Sb site, Sb(2) is bonded to one O(10), one O(13), one O(16), one O(20), one O(22), and one O(23) atom to form SbO6 octahedra that share  a cornercorner with one P(4)O4 tetrahedra,  a cornercorner with one P(5)O4 tetrahedra, corners with two equivalent P(1)O4 tetrahedra, and corners with two equivalent P(2)O4 tetrahedra. In the third Sb site, Sb(3) is bonded to one O(1), one O(11), one O(14), one O(21), one O(24), and one O(4) atom to form distorted SbO6 octahedra that share  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(6)O4 tetrahedra, corners with two equivalent P(3)O4 tetrahedra, and corners with two equivalent P(4)O4 tetrahedra. There are six inequivalent P sites. In the first P site, P(1) is bonded to one O(13), one O(23), one O(24), and one O(6) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(3)O6 octahedra and corners with two equivalent Sb(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 43-53°. In the second P site, P(2) is bonded to one O(10), one O(22), one O(7), and one O(9) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(1)O6 octahedra and corners with two equivalent Sb(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-45°. In the third P site, P(3) is bonded to one O(14), one O(4), one O(5), and one O(8) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(1)O6 octahedra and corners with two equivalent Sb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 36-51°. In the fourth P site, P(4) is bonded to one O(11), one O(17), one O(20), and one O(21) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(2)O6 octahedra and corners with two equivalent Sb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-49°. In the fifth P site, P(5) is bonded to one O(15), one O(16), one O(18), and one O(3) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(2)O6 octahedra and corners with two equivalent Sb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 38-43°. In the sixth P site, P(6) is bonded to one O(1), one O(12), one O(19), and one O(2) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(3)O6 octahedra and corners with two equivalent Sb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-48°. There are twenty-four inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one K(2), one Li(1), one Sb(3), and one P(6) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(6) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one K(1), one Sb(1), and one P(5) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Li(2), one Sb(3), and one P(3) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(3) atom. In the sixth O site, O(6) is bonded in a distorted linear geometry to one K(1), two equivalent K(2), one Li(1), and one P(1) atom. In the seventh O site, O(7) is bonded in a distorted single-bond geometry to one K(1), one K(3), and one P(2) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one K(2), one K(3), and one P(3) atom. In the ninth O site, O(9) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(2) atom. In the tenth O site, O(10) is bonded in a distorted T-shaped geometry to one Li(3), one Sb(2), and one P(2) atom. In the eleventh O site, O(11) is bonded in a 3-coordinate geometry to one Li(1), one Sb(3), and one P(4) atom. In the twelfth O site, O(12) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(6) atom. In the thirteenth O site, O(13) is bonded in a 2-coordinate geometry to one K(2), one Sb(2), and one P(1) atom. In the fourteenth O site, O(14) is bonded in a 2-coordinate geometry to one Li(2), one Sb(3), and one P(3) atom. In the fifteenth O site, O(15) is bonded in a distorted bent 150 degrees geometry to one Sb(1) and one P(5) atom. In the sixteenth O site, O(16) is bonded in a 3-coordinate geometry to one K(1), one Sb(2), and one P(5) atom. In the seventeenth O site, O(17) is bonded in a distorted single-bond geometry to two equivalent K(1), one Li(3), and one P(4) atom. In the eighteenth O site, O(18) is bonded in a 2-coordinate geometry to one K(3), two equivalent K(1), one Li(3), and one P(5) atom. In the nineteenth O site, O(19) is bonded in a distorted linear geometry to one K(2), one K(3), one Li(2), and one P(6) atom. In the twentieth O site, O(20) is bonded in a distorted T-shaped geometry to one Li(3), one Sb(2), and one P(4) atom. In the twenty-first O site, O(21) is bonded in a distorted bent 120 degrees geometry to one K(2), one Li(1), one Sb(3), and one P(4) atom. In the twenty-second O site, O(22) is bonded in a 3-coordinate geometry to one Li(3), one Sb(2), and one P(2) atom. In the twenty-third O site, O(23) is bonded in a 3-coordinate geometry to one K(1), one Sb(2), and one P(1) atom. In the twenty-fourth O site, O(24) is bonded in a 4-coordinate geometry to one K(2), one Li(2), one Sb(3), and one P(1) atom.
KLiSb(PO4)2 crystallizes in the triclinic P1 space group. There are three inequivalent K sites. In the first K site, K(1) is bonded in a 9-coordinate geometry to one O(16), one O(23), one O(3), one O(6), one O(7), two equivalent O(17), and two equivalent O(18) atoms. The K(1)-O(16) bond length is 2.91 Å. The K(1)-O(23) bond length is 2.92 Å. The K(1)-O(3) bond length is 3.16 Å. The K(1)-O(6) bond length is 2.91 Å. The K(1)-O(7) bond length is 3.15 Å. There is one shorter (2.86 Å) and one longer (2.92 Å) K(1)-O(17) bond length. There is one shorter (2.97 Å) and one longer (3.07 Å) K(1)-O(18) bond length. In the second K site, K(2) is bonded in a 8-coordinate geometry to one O(1), one O(13), one O(19), one O(21), one O(24), one O(8), and two equivalent O(6) atoms. The K(2)-O(1) bond length is 3.17 Å. The K(2)-O(13) bond length is 3.21 Å. The K(2)-O(19) bond length is 2.98 Å. The K(2)-O(21) bond length is 3.06 Å. The K(2)-O(24) bond length is 3.00 Å. The K(2)-O(8) bond length is 3.29 Å. There is one shorter (2.84 Å) and one longer (3.09 Å) K(2)-O(6) bond length. In the third K site, K(3) is bonded in a 4-coordinate geometry to one O(18), one O(19), one O(7), and one O(8) atom. The K(3)-O(18) bond length is 2.73 Å. The K(3)-O(19) bond length is 2.82 Å. The K(3)-O(7) bond length is 2.76 Å. The K(3)-O(8) bond length is 2.71 Å. There are three inequivalent Li sites. In the first Li site, Li(1) is bonded in a rectangular see-saw-like geometry to one O(1), one O(11), one O(21), and one O(6) atom. The Li(1)-O(1) bond length is 2.12 Å. The Li(1)-O(11) bond length is 1.96 Å. The Li(1)-O(21) bond length is 1.92 Å. The Li(1)-O(6) bond length is 1.79 Å. In the second Li site, Li(2) is bonded in a distorted rectangular see-saw-like geometry to one O(14), one O(19), one O(24), and one O(4) atom. The Li(2)-O(14) bond length is 2.02 Å. The Li(2)-O(19) bond length is 1.87 Å. The Li(2)-O(24) bond length is 2.12 Å. The Li(2)-O(4) bond length is 2.15 Å. In the third Li site, Li(3) is bonded in a 5-coordinate geometry to one O(10), one O(17), one O(18), one O(20), and one O(22) atom. The Li(3)-O(10) bond length is 2.30 Å. The Li(3)-O(17) bond length is 2.51 Å. The Li(3)-O(18) bond length is 1.99 Å. The Li(3)-O(20) bond length is 2.11 Å. The Li(3)-O(22) bond length is 2.25 Å. There are three inequivalent Sb sites. In the first Sb site, Sb(1) is bonded to one O(12), one O(15), one O(2), one O(3), one O(5), and one O(9) atom to form SbO6 octahedra that share  a cornercorner with one P(2)O4 tetrahedra,  a cornercorner with one P(3)O4 tetrahedra, corners with two equivalent P(5)O4 tetrahedra, and corners with two equivalent P(6)O4 tetrahedra. The Sb(1)-O(12) bond length is 2.00 Å. The Sb(1)-O(15) bond length is 2.01 Å. The Sb(1)-O(2) bond length is 2.01 Å. The Sb(1)-O(3) bond length is 2.02 Å. The Sb(1)-O(5) bond length is 1.98 Å. The Sb(1)-O(9) bond length is 2.00 Å. In the second Sb site, Sb(2) is bonded to one O(10), one O(13), one O(16), one O(20), one O(22), and one O(23) atom to form SbO6 octahedra that share  a cornercorner with one P(4)O4 tetrahedra,  a cornercorner with one P(5)O4 tetrahedra, corners with two equivalent P(1)O4 tetrahedra, and corners with two equivalent P(2)O4 tetrahedra. The Sb(2)-O(10) bond length is 2.14 Å. The Sb(2)-O(13) bond length is 2.11 Å. The Sb(2)-O(16) bond length is 2.17 Å. The Sb(2)-O(20) bond length is 2.14 Å. The Sb(2)-O(22) bond length is 2.25 Å. The Sb(2)-O(23) bond length is 2.15 Å. In the third Sb site, Sb(3) is bonded to one O(1), one O(11), one O(14), one O(21), one O(24), and one O(4) atom to form distorted SbO6 octahedra that share  a cornercorner with one P(1)O4 tetrahedra,  a cornercorner with one P(6)O4 tetrahedra, corners with two equivalent P(3)O4 tetrahedra, and corners with two equivalent P(4)O4 tetrahedra. The Sb(3)-O(1) bond length is 2.32 Å. The Sb(3)-O(11) bond length is 2.29 Å. The Sb(3)-O(14) bond length is 2.34 Å. The Sb(3)-O(21) bond length is 2.39 Å. The Sb(3)-O(24) bond length is 2.31 Å. The Sb(3)-O(4) bond length is 2.19 Å. There are six inequivalent P sites. In the first P site, P(1) is bonded to one O(13), one O(23), one O(24), and one O(6) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(3)O6 octahedra and corners with two equivalent Sb(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 43-53°. The P(1)-O(13) bond length is 1.58 Å. The P(1)-O(23) bond length is 1.57 Å. The P(1)-O(24) bond length is 1.56 Å. The P(1)-O(6) bond length is 1.51 Å. In the second P site, P(2) is bonded to one O(10), one O(22), one O(7), and one O(9) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(1)O6 octahedra and corners with two equivalent Sb(2)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-45°. The P(2)-O(10) bond length is 1.57 Å. The P(2)-O(22) bond length is 1.57 Å. The P(2)-O(7) bond length is 1.51 Å. The P(2)-O(9) bond length is 1.60 Å. In the third P site, P(3) is bonded to one O(14), one O(4), one O(5), and one O(8) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(1)O6 octahedra and corners with two equivalent Sb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 36-51°. The P(3)-O(14) bond length is 1.56 Å. The P(3)-O(4) bond length is 1.58 Å. The P(3)-O(5) bond length is 1.60 Å. The P(3)-O(8) bond length is 1.51 Å. In the fourth P site, P(4) is bonded to one O(11), one O(17), one O(20), and one O(21) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(2)O6 octahedra and corners with two equivalent Sb(3)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-49°. The P(4)-O(11) bond length is 1.56 Å. The P(4)-O(17) bond length is 1.52 Å. The P(4)-O(20) bond length is 1.60 Å. The P(4)-O(21) bond length is 1.55 Å. In the fifth P site, P(5) is bonded to one O(15), one O(16), one O(18), and one O(3) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(2)O6 octahedra and corners with two equivalent Sb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 38-43°. The P(5)-O(15) bond length is 1.58 Å. The P(5)-O(16) bond length is 1.56 Å. The P(5)-O(18) bond length is 1.51 Å. The P(5)-O(3) bond length is 1.58 Å. In the sixth P site, P(6) is bonded to one O(1), one O(12), one O(19), and one O(2) atom to form PO4 tetrahedra that share  a cornercorner with one Sb(3)O6 octahedra and corners with two equivalent Sb(1)O6 octahedra. The corner-sharing octahedral tilt angles range from 37-48°. The P(6)-O(1) bond length is 1.55 Å. The P(6)-O(12) bond length is 1.58 Å. The P(6)-O(19) bond length is 1.52 Å. The P(6)-O(2) bond length is 1.58 Å. There are twenty-four inequivalent O sites. In the first O site, O(1) is bonded in a 3-coordinate geometry to one K(2), one Li(1), one Sb(3), and one P(6) atom. In the second O site, O(2) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(6) atom. In the third O site, O(3) is bonded in a distorted bent 150 degrees geometry to one K(1), one Sb(1), and one P(5) atom. In the fourth O site, O(4) is bonded in a 3-coordinate geometry to one Li(2), one Sb(3), and one P(3) atom. In the fifth O site, O(5) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(3) atom. In the sixth O site, O(6) is bonded in a distorted linear geometry to one K(1), two equivalent K(2), one Li(1), and one P(1) atom. In the seventh O site, O(7) is bonded in a distorted single-bond geometry to one K(1), one K(3), and one P(2) atom. In the eighth O site, O(8) is bonded in a distorted single-bond geometry to one K(2), one K(3), and one P(3) atom. In the ninth O site, O(9) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(2) atom. In the tenth O site, O(10) is bonded in a distorted T-shaped geometry to one Li(3), one Sb(2), and one P(2) atom. In the eleventh O site, O(11) is bonded in a 3-coordinate geometry to one Li(1), one Sb(3), and one P(4) atom. In the twelfth O site, O(12) is bonded in a bent 150 degrees geometry to one Sb(1) and one P(6) atom. In the thirteenth O site, O(13) is bonded in a 2-coordinate geometry to one K(2), one Sb(2), and one P(1) atom. In the fourteenth O site, O(14) is bonded in a 2-coordinate geometry to one Li(2), one Sb(3), and one P(3) atom. In the fifteenth O site, O(15) is bonded in a distorted bent 150 degrees geometry to one Sb(1) and one P(5) atom. In the sixteenth O site, O(16) is bonded in a 3-coordinate geometry to one K(1), one Sb(2), and one P(5) atom. In the seventeenth O site, O(17) is bonded in a distorted single-bond geometry to two equivalent K(1), one Li(3), and one P(4) atom. In the eighteenth O site, O(18) is bonded in a 2-coordinate geometry to one K(3), two equivalent K(1), one Li(3), and one P(5) atom. In the nineteenth O site, O(19) is bonded in a distorted linear geometry to one K(2), one K(3), one Li(2), and one P(6) atom. In the twentieth O site, O(20) is bonded in a distorted T-shaped geometry to one Li(3), one Sb(2), and one P(4) atom. In the twenty-first O site, O(21) is bonded in a distorted bent 120 degrees geometry to one K(2), one Li(1), one Sb(3), and one P(4) atom. In the twenty-second O site, O(22) is bonded in a 3-coordinate geometry to one Li(3), one Sb(2), and one P(2) atom. In the twenty-third O site, O(23) is bonded in a 3-coordinate geometry to one K(1), one Sb(2), and one P(1) atom. In the twenty-fourth O site, O(24) is bonded in a 4-coordinate geometry to one K(2), one Li(2), one Sb(3), and one P(1) atom.