Abstract
The tetrameric Cu(β‐diketonate) alkoxide complex [Cu(thd)(OCH~2~CH~2~OCH~3~)]~4~ (thd = 2,2,6,6‐tetramethyl‐3,5‐heptanedionate; 1a) reacts with the alkaline earth metal alkoxides [M(OCH~2~CH~2~OCH~3~)~2~] (M = Ca, 2a; M = Sr, 2b; M = Ba, 2c) to yield the heteronuclear compounds [Cu~2~M(thd)~3~(OCH~2~CH~2~OCH~3~)~3~] (M = Ca, 6a; M = Sr, 6b). These heterometallic complexes were also obtained in the reaction of 1a and the mixed Ca and Sr complexes of β‐diketonate‐alkoxide [M~x~(thd)~y~(OCH~2~CH~2~OCH~3~)~2x−y~] (M = Ca, x = 7, y = 6, 3; M = Sr, x = 5, y = 3, 4), respectively. In comparison, 1a reacts with the analogous [Ba(thd)(OCH~2~CH~2~OCH~3~)] (5a) to yield a[Ba~2~Cu~2~(thd)~4~(OCH~3~)~4~(HOCH~2~CH~2~OCH~3~)~2~] species (8a.) The in situ prepared mixed‐ligand Ba Compounds [Ba(thd)OR)] (R = CH~2~CH~2~OCH~2~CH~2~OCH~3~, (5b); R = CH~2~CH~2~CH~2~OCH~3~ (5c) react with the corresponding Cu complexes [Cu(thd)(OR)]~n~ (R = CH~2~CH~2~OCH~2~CH~2~OCH~3~), n = 4 (1b); R = CH~2~CH~2~OCH~2~CH~2~OCH~3~ (8b); R = CH~2~CH~2~CH~2~OCH~3~ (8c). However, [Cu(hfd)(OCH~2~CH~2~OCH~3~)]~4~ (hfd = 1,1,1,5,5,5,‐hexafluoroacetylacetonate; 1e) is converted in the presence of 2a–c to the simple metathesis products [M(hfd)~2~] (M = Ca, Sr, Ba) and [Cu(OCH~2~CH~2~OCH~3~)~2~]. Crystalline [Ba~2~Cu~2~(hfd)~2~(thd)~2~(OCH~2~CH~2~CH~2~OCH~3~)~4~(HOCH~2~CH~2~CH~2~OCH~3~)~2~] (9) was isolated from the reaction of 1a with in situ prepared [Ba((hfd)OCH~2~CH~2~CH~2~OCH~3~)] (5d) in 2‐, methoxyethanol. X‐Ray crystallographic structure determinations are reported for 6a, 6b, 8b, and 8c.