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Three new compounds of the Cs Ln [P 2 Se 6 ] family with  Ln  = Ce, Sm and Er have been prepared and structurally characterized. Plate-shaped, amber-colored single crystals of these cesium lanthanoid(III) hexaselenodiphosphates(IV) were obtained by heating stoichiometric amounts of  Ln , P and Se with CsCl as a reactive flux in fused silica ampoules at 800 °C for four days. CsCe[P 2 Se 6 ] crystallizes monoclinically in space group  P 2 1 / c  with  a  = 1297.86(9),  b  = 776.24(5),  c  = 1198.43(8) pm,  β  = 106.589(3)° and  Z  = 4. The structure is isotypic with that of KLa[P 2 Se 6 ], the Cs +  cations being ten-fold coordinated by selenium atoms to form double layers of condensed [CsSe 10 ] 19−  polyhedra. Ce 3+  resides in a nine-fold coordination and the [CeSe 9 ] 15−  polyhedra also form double layers parallel to (100). CsSm[P 2 Se 6 ] crystallizes in the orthorhombic space group  P 2 1 2 1 2 1  with  a  = 688.67(5),  b  = 754.48(5),  c  = 2215.21(15) pm and  Z  = 4. Its structure is isotypic with that of KY[P 2 Se 6 ] and the Cs +  cations reside in an eleven-fold coordination of selenium atoms constituting monolayers of condensed [CsSe 11 ] 21−  polyhedra within the (001) plane. Sm 3+  exhibits an eight-fold coordination sphere of selenium atoms and the [SmSe 8 ] 13−  polyhedra are also linked to build up parallel monolayers. CsEr[P 2 Se 6 ] crystallizes in the monoclinic space group  P 2 1 / c  again, but forms its own structure type with the lattice parameters  a  = 753.81(5),  b  = 1281.92(9),  c  = 1276.47(9) pm and  β  = 106.898(3)° and  Z  = 4. The Cs +  cations are twelve-fold coordinated by selenium atoms and erects a three-dimensional framework of condensed [CsSe 12 ] 23−  polyhedra. The Er 3+  cations show seven selenium atoms as neighbors and the [ErSe 7 ] 11−  polyhedra are edge-connected to form discrete dimers [Er 2 Se 12 ] 18− . All three structures have similar ethane-like [P 2 Se 6 ] 4–  anions in staggered conformation with bond lengths of 219–226 pm for  d (P1–P2) and 213–222 pm for  d (P–Se), which connect the Cs +  and  Ln   3+   coordination polyhedra into three-dimensional crystal structures.

Three of a kind? The non-isotypic triple CsCe[P 2 Se 6 ], CsSm[P 2 Se 6 ] and CsEr[P 2 Se 6 ]