SYNTHESIS AND CHARACTERIZATION OF VOLATILE MIXED-METAL YTTRIUM-BARIUM, BARIUM-COPPER AND YTTRIUM-COPPER BETA-DIKETONATOFLUOROISOPROPOXIDES - MOLECULAR-STRUCTURE OF BAY2[MU-OCH(CF3)(2)](4)(THD)4
F. Labrize et al., SYNTHESIS AND CHARACTERIZATION OF VOLATILE MIXED-METAL YTTRIUM-BARIUM, BARIUM-COPPER AND YTTRIUM-COPPER BETA-DIKETONATOFLUOROISOPROPOXIDES - MOLECULAR-STRUCTURE OF BAY2[MU-OCH(CF3)(2)](4)(THD)4, Polyhedron, 15(16), 1996, pp. 2707-2718
Heterometallic complexes [YBa2(HFIP)(7)(THF)(3)] (1) and [BaCu(HFIP)(4
)(DME)(2)] (2); HFIP = 1,1,1,3,3,3-hexafluoro-2-propoxide) were obtain
ed by metathesis reactions between YCl3 or CuCl2 and ''Ba(HFIP)(2)'' o
btained in situ or by using the isolated barium hexafluoroisopropoxide
[Ba-5(OH)(HFIP)(9)(THF)(4)(H2O)]. The fluoroisopropoxides [Y(HFIP)(3)
(THF)(3)] (3) and [Y-2(HFIP)(2)(thd)(4)] (4) are alternative yttrium s
ources. Volatile mixed-metal complexes [Y2Ba(HFIP)(4)(thd)(4)] (5), [B
aCu2(HFIP)(4)(thd)(2)] (6) and [YCu (HFIP)(thd)] (7); thdH = 2,2,6,6-t
etramethyl-3,5-heptanedione) were synthesized by reacting 1, 2 or 3 wi
th tetramethylheptanedionates of yttrium, copper and barium or directl
y with Hthd for 5 and 6. An alternative route to 5 was the reaction of
4 with [Ba-5(OH)(HFIP)(9)(THF)(4)(H2O)]. The compounds were all obtai
ned in high yields. They were characterized by elemental analysis, mas
s spectrometry, NMR (H-1, F-19, C-13 {H-1}) and ESR spectroscopy, as w
ell as vapour pressure measurements and single-crystal X-ray diffracti
on for 5. The volatilities of compounds 5, 6 and 7 are in the range 15
0-170 degrees C/10(-3) Torr and are the best encountered among mixed-m
etal compounds containing barium, yttrium and copper. Copyright (C) 19
96 Elsevier Science Ltd