Journal
JOURNAL OF COORDINATION CHEMISTRY
Volume 68, Issue 11, Pages 1890-1902Publisher
TAYLOR & FRANCIS LTD
DOI: 10.1080/00958972.2015.1035653
Keywords
Heterometallic complexes; Metal beta-diketonates; Bimetallic precursors; Volatile metal-organic complexes
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Preparation of volatile heterometallic precursors is a significant step on the way to advanced multicomponent materials. Study of molecular transformations in solution upon precursor synthesis is of importance to optimize the preparation of the stable solid product of desired composition. Two new volatile heterobimetallic complexes, cis-PdL2*Pb(hfa)(2) and cis-CuL2*Pb(hfa)(2), were obtained (L=2-methoxy-2,6,6-trimethylheptane-3,5-dionate, hfa=1,1,1,5,5,5-hexafluoropentane-2,4-dionate) under cocrystallization of trans-bis-beta-diketonates of Pd(II) and Cu(II) with Pb(hfa)(2) from organic solvents. Crystals of these compounds are built of discrete bimetallic molecules where transition metal complex isomerized from trans-to-cis form. Complexation followed by isomerization was studied by solution NMR. The bimetallic molecular species were formed early in solution. Enthalpy and activation energy of isomerization were estimated to be 49 and 93kJmol(-1), respectively. A new synthesis technique of Pd(II) beta-diketonates which is distinguished by simplicity and selectivity as well as the crystal structure of trans-PdL2 is described. Volatility of all obtained compounds was confirmed by thermogravimetric analysis and fractional sublimation in vacuum; Pd-containing heterobimetallic complex appeared to be more volatile than both the initial monometallic complexes and Cu-containing complex.
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