Reaction of Ti(OiPr)4 with various bis(β-diketones) and bis(β-ketoesters) (LH2) results in the formation of dimeric complexes [Ti(OiPr)2L]2, where each metal centre is coordinated by two terminal OiPr ligands and two bridging β-diketonate or β-ketoesterate groups (L). Macrocycles containing two M(OiPr)2 moieties are thus formed. Reaction of Zr(OiPr)4 with the same bis(β-diketones) and bis(β-ketoesters) results in different compounds, depending on the organic spacer connecting the two functional groups. With shorter spacers, the compounds [ZrL(OiPr)2]2·2iPrOH are obtained, with the same structures as the corresponding titanium complexes. With longer spacers, however, complexes with a higher degree of substitution are formed, such as (ZrL2)2 and Zr2L3(OiPr)2·2iPrOH. The molecular weight and structure of all compounds was elucidated by ESI-MS. MS/MS of the corresponding [M+Na]+ precursor ions confirmed the proposed structures based on structure-specific product ions. Solution NMR experiments and DFT calculations additionally supported the proposed structures.
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