Premium
Single Crystals of CaNa[ReO 4 ] 3 : Serendipitous Formation and Systematic Characterization
Author(s) -
Conrad Maurice,
Schleid Thomas
Publication year - 2019
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.201900189
Subject(s) - octahedron , crystallography , crystal structure , chemistry , microcrystalline , trigonal prismatic molecular geometry , hexagonal crystal system , salt metathesis reaction , metathesis , organic chemistry , polymerization , polymer
In an attempt to crystallize Ce[ReO 4 ] 4 · x H 2 O from aqueous solutions of equimolar amounts of Ce[SO 4 ] 2 and Ba[ReO 4 ] 2 via salt‐metathesis the serendipitous formation of colorless, transparent, rod‐shaped single crystals of CaNa[ReO 4 ] 3 was observed as a result of calcium and sodium impurities within the improperly deionized water used. Structure analysis by X‐ray diffraction lead to the conclusion that the title compound crystallizes in the ThCd[MoO 4 ] 3 structure type with the hexagonal space group P 6 3 / m and the lattice parameters a = 991.74(6) pm, c = 636.53(4) pm, c/a = 0.642 for Z = 2. The crystal structure contains purely oxygen surrounded and crystallographically unique cations, namely Ca 2+ in tricapped trigonal prismatic ( d (Ca–O) = 6 × 249 pm + 3 × 254 pm), Na + in octahedral ( d (Na–O) = 6 × 241 pm), and Re 7+ in tetrahedral coordination ( d (Re–O) = 171–173 pm). Furthermore, it was possible to yield an almost phase‐pure microcrystalline powder of the title compound from a melt of equimolar amounts of Na[ReO 4 ] and Ca[ReO 4 ] 2 stemming from aquatically obtained precursors.