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The chlorides Na 3 MCl 6 (M EuLu, Y, Sc): Synthesis, crystal structures, and thermal behaviour
Author(s) -
Meyer Gerd,
Peter Ax Studienrat,
Schleid Thomas,
Irmler Manfred
Publication year - 1987
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.19875541104
Subject(s) - cryolite , crystallography , crystal structure , molar ratio , chemistry , lattice constant , molar volume , materials science , diffraction , aluminium , thermodynamics , physics , biochemistry , optics , catalysis , organic chemistry
Single crystals of Na 3 ErCl 6 were obtained via the metallothermic reduction of ErCl 3 with Na. The crystal structure is that of the mineral cryolite with a = 684.54(4), b = 725.18(4), c = 1012.39(6) pm, β = 90.768(5)°, Z = 2, space group P2 1 /n. Two applicable synthetic routes to pure powder samples of the chlorides Na 3 MCl 6 (M EuLu, Y, Sc) are described. With M DyLu, Y, Sc, these are isotypic with Na 3 ErCl 6 while those with M Eu, Gd, Tb adopt a „stuffed” LiSbF 6 ‐type structure. The dimorphism of Na 3 GdCl 6 and dependence of the lattice constants and the molar volume upon temperature has been investigated: At 205°C, a first‐order phase transition from the stuffed LiSbF 6 ‐type Na 3 GdCl 6 ‐I to the cryolite‐type Na 3 GdCl 6 ‐II occurs exhibiting a 3.71% negative molar volume discontinuity.