TY - JOUR
T1 - Crystal structure of [CF3CFC(CF3)Ag]4 and its use as a chemical vapor deposition precursor for silver films
AU - Jeffries, Patrick M.
AU - Wilson, Scott R.
AU - Girolami, Gregory S.
N1 - Funding Information:
We thank the Department of Energy (Contract DE-AC 02-76 ER 1198) and the National Science Foundation (DMR 88-09854) through the Science and Technology Center for Superconductivity for funding . XPS and XPD were carried out in the Center for Microanalysis of Materials, University of Illinois, which is supported by the US Department of Energy under contract DE-AC 02-76ER 01198 . SEM was performed at the Center for Electron Microscopy at the University of Illinois . We particularly thank Teresa Prussak-Wieckowska of the University of Illinois X-ray Crystallographic Laboratory for assistance with the crystallographic studies . P .M .J . is the recipient of a University of Illinois Department of Chemistry Fellowship . G .S .G . acknowledges an A .P . Sloan Foundation Research Fellowship and a Henry and Camille Dreyfus Teacher-Scholar Award (1988-1993) .
PY - 1993/5/4
Y1 - 1993/5/4
N2 - Silver films have been prepared by the metal-organic chemical vapor deposition of perfluoro-1-methyl-1-propenylsilver tetramer, [CF3CFC(CF3)Ag]4, at 275°C and 10-4 Torr; the silver films contain only traces (< 1%) of fluorine and oxygen and no carbon. The principal organic byproducts formed during deposition are trans-CF3CFCH(CF3) (50%) and CF3CCCF3 (40%). It is argued that silver metal is produced by elimination of CF3CCCF3 from trans-[CF3CFC(CF3)Ag]4 to form silver(I) fluoride, which defluorinates to form silver metal. The crystal structure of trans-[CF3CFC(CF3)Ag]4 was determined and reveals that this compound is a tetramer that consists of a square plane of silver atoms in which each edge is bridged by a trans-perfluoro-1-methyl-1-propenyl ligand. The average distances and angles are: AgAg = 2.761 Å, AgC = 2.19 Å, AgCAg = 78.3° and CAgC = 166.7°. Crystal data: monoclinic, space group P21/c, a = 9.480(5) Å, b = 15.589(6) Å, c = 18.919(4) Å, β = 90.27(3)°, V = 2796(4) Å3, Z = 4, Rf = 0.070, and RwF = 0.089 on 433 variables and 3617 data with I > 2.58 σ(I).
AB - Silver films have been prepared by the metal-organic chemical vapor deposition of perfluoro-1-methyl-1-propenylsilver tetramer, [CF3CFC(CF3)Ag]4, at 275°C and 10-4 Torr; the silver films contain only traces (< 1%) of fluorine and oxygen and no carbon. The principal organic byproducts formed during deposition are trans-CF3CFCH(CF3) (50%) and CF3CCCF3 (40%). It is argued that silver metal is produced by elimination of CF3CCCF3 from trans-[CF3CFC(CF3)Ag]4 to form silver(I) fluoride, which defluorinates to form silver metal. The crystal structure of trans-[CF3CFC(CF3)Ag]4 was determined and reveals that this compound is a tetramer that consists of a square plane of silver atoms in which each edge is bridged by a trans-perfluoro-1-methyl-1-propenyl ligand. The average distances and angles are: AgAg = 2.761 Å, AgC = 2.19 Å, AgCAg = 78.3° and CAgC = 166.7°. Crystal data: monoclinic, space group P21/c, a = 9.480(5) Å, b = 15.589(6) Å, c = 18.919(4) Å, β = 90.27(3)°, V = 2796(4) Å3, Z = 4, Rf = 0.070, and RwF = 0.089 on 433 variables and 3617 data with I > 2.58 σ(I).
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U2 - 10.1016/0022-328X(93)80124-T
DO - 10.1016/0022-328X(93)80124-T
M3 - Article
AN - SCOPUS:0001030807
SN - 0022-328X
VL - 449
SP - 203
EP - 209
JO - Journal of Organometallic Chemistry
JF - Journal of Organometallic Chemistry
IS - 1-2
ER -