Synthesis and characterization of volatile mixed-metal yttrium-barium, barium-copper and yttrium-copper β-diketonatofluoroisopropoxides. Molecular structure of BaY2[μ-OCH(CF3)2]4(thd)4

Autor: Pascal Tobaly, Florence Labrize, Sabine Halut, Jean-Claude Daran, Liliane G. Hubert-Pfalzgraf
Rok vydání: 1996
Předmět:
Zdroj: Polyhedron. 15:2707-2718
ISSN: 0277-5387
DOI: 10.1016/0277-5387(95)00557-9
Popis: Heterometallic complexes [YBa 2 (HFIP) 7 (THF) 3 ] ( 1 ) and [BaCu(HFIP) 4 (DME) 2 ] ( 2 ); HFIP = 1,1,1,3,3,3-hexafluoro-2-propoxide) were obtained by metathesis reactions between YCl 3 or CuCl 2 and “Ba(HFIP) 2 ” obtained in situ or by using the isolated barium hexafluoroisopropoxide [Ba 5 (OH)(HFIP) 9 (THF) 4 (H 2 O)]. The fluoroisopropoxides [Y(HFIP) 3 (THF) 3 ] ( 3 ) and [Y 2 (HFIP) 2 (thd) 4 ] ( 4 ) are alternative yttrium sources. Volatile mixed-metal complexes [Y 2 Ba(HFIP) 4 (thd) 4 ] ( 5 ), [BaCu 2 (HFIP) 4 (thd) 2 ] ( 6 ) and [YCu (HFIP)(thd)] ( 7 ); thdH = 2,2,6,6-tetramethyl-3,5-heptanedione) were synthesized by reacting 1 , 2 or 3 with tetramethylheptanedionates of yttrium, copper and barium or directly with Hthd for 5 and 6 . An alternative route to 5 was the reaction of 4 with [Ba 5 (OH)(HFIP) 9 (THF) 4 (H 2 O)]. The compounds were all obtained in high yields. They were characterized by elemental analysis, mass spectrometry, NMR ( 1 H, 19 F, 13 C { 1 H}) and ESR spectroscopy, as well as vapour pressure measurements and single-crystal X-ray diffraction for 5 . The volatilities of compounds 5 , 6 and 7 are in the range 150–170°C/10 −3 Torr and are the best encountered among mixed-metal compounds containing barium, yttrium and copper.
Databáze: OpenAIRE