SYNTHESIS AND CHARACTERIZATION OF (BETA-DIKETONATE)(7-NORBORNADIENYL ACETATE)COPPER(I) COMPLEXES, SINGLE-CRYSTAL STRUCTURE OF (HFAC)CU(7-ACO-NBD)

摘要

Copper(I) complexes of general formula (beta-diketonate)Cu(7-AcO-NBD), where 7-AcO-NBD = 7-norbornadienyl acetate and beta-diketonate = 1,1,1,5,5,5-hexafluoro-2,4-pentanedionate (1), 1,1,1-trifluoro-2,4-pentanedionate (2), 2,4-pentanedionate (3), 4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedionate (4), 4,4,4-trifluoro-1-phenyl-1,3-butanedionate (5), were prepared from reactions of CuCl with Na(beta-diketonate) in the presence of 7-AcO-NBD. All compounds were characterized by elemental analyses, H-1, C-13, F-19 NMR and IR spectra. Single-crystal strucutre of compound 1 was determined by X-ray diffraction analysis that showed a mononuclear copper species with coordination of a chelating beta-diketonate ligand through two oxygen atoms and the 7-AcO-NBD through its C=C double bond and an oxygen atom in the solid state. For compound 1, the crystal data are: triclinic, space group , a = 5.4519(14) Angstrom, b = 11.852(3) Angstrom, c = 13.304(3) Angstrom, alpha = 74.721(20)degrees, beta = 80.220(20)degrees, gamma = 76.848(19)degrees, Z = 2, R(F) = 0.060 and R(W) = 0.064. Hot-wall chemical vapor deposition experiments revealed that compound 1 is suitable as a precursor for deposition of copper films in the temperature range 170-260 degrees C. [References: 28]