Synthesis and characterization of calcium β-diketonate complexes. X-Ray crystal and molecular structures of: [{Ca(tmhd)2}2(18-crown-6)], [Ca(dpp)2(thf)2] and [Ca(dpp)2(triglyme)]?

Dalton Transactions Pub Date: 2010-07-14 DOI: 10.1039/C001854F

Abstract

Reactions of 2,2,6,6-tetramethyl-3,5-heptanedione (Htmhd), 1,1,1,5,5,5-hexafluoro-2,4-pentanedione (Hhfa) or 1,3-diphenyl-1,3-propanedione (Hdpp) with calcium methoxide in hexane or toluene afford the corresponding known oligomeric β-diketonates: [Ca3(tmhd)6], [{Ca(hfa)2}n] and [{Ca(dpp)2}n]. The complexes react with tetrahydrofuran, 2,5,8,11-tetraoxadodecane (triglyme) or 1,4,7,10,13,16-hexaoxacyclooctadecane (18-crown-6) leading to the formation of the new mononuclear [Ca(dpp)2(thf)2], [Ca(dpp)2(triglyme)] and dinuclear [{Ca(dpp)2}2(18-crown-6)] and [{Ca(tmhd)2}2(18-crown-6)] adducts. The obtained complexes were characterized by elemental analyses, IR, 1H and 13C NMR spectroscopies; moreover, single crystal X-ray diffraction measurements were also carried out for: [{Ca(tmhd)2}2(18-crown-6)], [Ca(dpp)2(thf)2] and [Ca(dpp)2(triglyme)].

Graphical abstract: Synthesis and characterization of calcium β-diketonate complexes. X-Ray crystal and molecular structures of: [{Ca(tmhd)2}2(18-crown-6)], [Ca(dpp)2(thf)2] and [Ca(dpp)2(triglyme)]
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