Synthesis and Characterization of (.beta.-Diketonate)(7-tert-butoxynorbornadiene)copper(I) Compounds, a Series of New Copper CVD Precursors
Resource
Organometallics 14 (6): 2641-2648
Journal
Organometallics
Pages
2641-2648
Date Issued
1995
Date
1995
Author(s)
Abstract
Organocopper compounds of the general formula (β-diketonate)Cu(7-t-BuO-NBD) where 7-t-BuO-NBD = 7-tert-butoxynorbornadiene and β-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), and 2,2-dimethyl-6,6,7,7,8,8,8-heptafluoro-3,5-octanedionate (6) were prepared by reaction of CuCl with Na(β-diketonate) in the presence of 7-t-BuO-NBD. All compounds were characterized by elemental analyses and 1H, 13C, and 19F NMR, IR, and mass spectra. Singlecrystal structures of compounds 1, 4, and 5 were determined by X-ray diffraction analyses that showed mononuclear copper species with coordination of a chelating β-diketonate ligand through two oxygen atoms and the 7-t-BuO-NBD through one C=C double bond and an oxygen atom in the solid state. Variable-temperature 1H NMR spectral data of compound 2 in the solution are consistent with this structural nature. Hot-wall chemical vapor deposition experiments revealed that compound 1 is suitable as a precursor to deposit copper films in the temperature range 200—260 °C. Crystallographic data for compounds 1, 4, and 5: (hfac)Cu(7-t-BuO-NBD) (1) crystallizes in monoclinic system, space group P21/c, a = 8.923(1) Å, b = 19.558(4) Å, c = 10.495(3) Å, β = 90.45(2)°, V = 1831.3(7) Å3, Z = 4. (Ttfac)Cu(7-t-BuO-NBD) (4) crystallizes in monoclinic system, space group P21/n, a = 10.689(6) Å, b = 9.712(4) Å, c = 19.323(4) Å, = 97.22(3)°, V = 1990.2(15) Å3, Z = 4. (Btfac)Cu(7-t-BuO-NBD) (5) crystallizes in triclinic system, space group P1, a = 9.617(1) Å, b = 9.894(4) Å, c = 11.322(2) Å, α = 104.57(2)°, β = 95.50(1)°, γ = 104.76(3)°, V = 993.4(5) A3, Z = 2. © 1995, American Chemical Society. All rights reserved.
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journal article
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