KSbF4 crystallizes in the orthorhombic Pmmn space group. There are two inequivalent K sites. In the first K site, K(1) is bonded in a distorted body-centered cubic geometry to two equivalent F(1), two equivalent F(4), and four equivalent F(5) atoms. In the second K site, K(2) is bonded in a 10-coordinate geometry to two equivalent F(2), two equivalent F(3), two equivalent F(5), and four equivalent F(4) atoms. There are two inequivalent Sb sites. In the first Sb site, Sb(1) is bonded to one F(2), two equivalent F(3), and two equivalent F(4) atoms to form distorted corner-sharing SbF5 square pyramids. In the second Sb site, Sb(2) is bonded to one F(1), two equivalent F(3), and two equivalent F(5) atoms to form distorted corner-sharing SbF5 square pyramids. There are five inequivalent F sites. In the first F site, F(4) is bonded to one K(1), two equivalent K(2), and one Sb(1) atom to form a mixture of distorted corner and edge-sharing FK3Sb tetrahedra. In the second F site, F(5) is bonded to one K(2), two equivalent K(1), and one Sb(2) atom to form a mixture of distorted corner and edge-sharing FK3Sb tetrahedra. In the third F site, F(1) is bonded in a distorted trigonal non-coplanar geometry to two equivalent K(1) and one Sb(2) atom. In the fourth F site, F(2) is bonded in a single-bond geometry to two equivalent K(2) and one Sb(1) atom. In the fifth F site, F(3) is bonded in a distorted T-shaped geometry to one K(2), one Sb(1), and one Sb(2) atom.
KSbF4 crystallizes in the orthorhombic Pmmn space group. There are two inequivalent K sites. In the first K site, K(1) is bonded in a distorted body-centered cubic geometry to two equivalent F(1), two equivalent F(4), and four equivalent F(5) atoms. Both K(1)-F(1) bond lengths are 2.74 Å. Both K(1)-F(4) bond lengths are 2.68 Å. There are two shorter (2.72 Å) and two longer (2.80 Å) K(1)-F(5) bond lengths. In the second K site, K(2) is bonded in a 10-coordinate geometry to two equivalent F(2), two equivalent F(3), two equivalent F(5), and four equivalent F(4) atoms. Both K(2)-F(2) bond lengths are 2.97 Å. Both K(2)-F(3) bond lengths are 2.85 Å. Both K(2)-F(5) bond lengths are 2.91 Å. There are two shorter (2.65 Å) and two longer (2.79 Å) K(2)-F(4) bond lengths. There are two inequivalent Sb sites. In the first Sb site, Sb(1) is bonded to one F(2), two equivalent F(3), and two equivalent F(4) atoms to form distorted corner-sharing SbF5 square pyramids. The Sb(1)-F(2) bond length is 1.96 Å. Both Sb(1)-F(3) bond lengths are 2.25 Å. Both Sb(1)-F(4) bond lengths are 2.01 Å. In the second Sb site, Sb(2) is bonded to one F(1), two equivalent F(3), and two equivalent F(5) atoms to form distorted corner-sharing SbF5 square pyramids. The Sb(2)-F(1) bond length is 1.97 Å. Both Sb(2)-F(3) bond lengths are 2.22 Å. Both Sb(2)-F(5) bond lengths are 2.02 Å. There are five inequivalent F sites. In the first F site, F(4) is bonded to one K(1), two equivalent K(2), and one Sb(1) atom to form a mixture of distorted corner and edge-sharing FK3Sb tetrahedra. In the second F site, F(5) is bonded to one K(2), two equivalent K(1), and one Sb(2) atom to form a mixture of distorted corner and edge-sharing FK3Sb tetrahedra. In the third F site, F(1) is bonded in a distorted trigonal non-coplanar geometry to two equivalent K(1) and one Sb(2) atom. In the fourth F site, F(2) is bonded in a single-bond geometry to two equivalent K(2) and one Sb(1) atom. In the fifth F site, F(3) is bonded in a distorted T-shaped geometry to one K(2), one Sb(1), and one Sb(2) atom.