- Alkene and carbon monoxide derivatives of copper(I) and silver(I) β-diketonates
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In the presence of CO or various alkenes and dienes, Cu2O will react with certain partially fluorinated β-diketones (Hdiket) to form complexes of the type [Cu(diket)]nLm (L = CO, alkene, or diene; n and m = 1 or 2). The complexes of CO or light olefins are unstable and subject to disproportionation, but nonvolatile alkenes and dienes form isolable compounds. Cyclooctatetraene (COT) forms a complex with the composition Cu2(COT)(hfacac)2 (Hhfacac = 1,1,1,5,5,5-hexafluoro-2,4-pentanedione), the structure of which was determined by single-crystal X-ray diffraction. The material crystallizes in the triclinic space group P1 with a = 8.121 (2) A?, b = 9.555 (2) A?, c = 14.756 (3) A?, α = 86.67 (1)°, β = 76.45 (1)°, and Z = 2. A combination of direct methods and Fourier techniques were used in the structural analysis and full-matrix least-squares refinement with 340 variables has converged to final R values of R = 0.084 and Rw = 0.090 for 1914 reflections. The structure consists of a central Cyclooctatetraene (COT) ring, one copper atom above the ring, a second copper atom below the ring, and a hexafluoroacetylacetonate (hfacac) group coordinated to each copper. Each of the copper atoms is disordered between two positions in a plane roughly perpendicular to the hfacac group to which it is coordinated. The two disorder positions are nearly equidistant from the hfacac oxygen atoms but are within bonding distance of opposite double bonds in the COT ligand. The geometry around the copper atoms is trigonal.
- Doyle,Eriksen,Van Engen
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p. 830 - 835
(2008/10/08)
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