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Multinuclear NMR and Thermal Studies of New Silver(I) Silylated Carboxylates with Triphenylphosphine

Szłyk E., Szymańska I., Szczęsny R.

Polish Journal of Chemistry

2005

Vol. 79 / nr 4

627-635

Me3SiCH2COOAg, [Ag(Me3SiCH2COO)(PPh3)] and [Ag(Me3SiCH2CH2COO)(PPh3)] were prepared and characterized in solution by 1H, 13C, 29Si, 31P and 29Si, 31P CPMAS NMR. Spectral analysis suggests bidentate bridging carboxylates and monodentately bonded PPh3 in solution and in the solid state. Two crystallographically inequivalent molecules of PPh3 appeared in the solid state, what is evident from 31P CPMAS NMR. Thermal studies of both complexes demonstrate two stage decomposition process (exothermic followed by endothermic) with formation of metallic silver in the range 483-548 K. TGA/IR and MS studies of Me3SiCH2COOAg and [Ag(Me3SiCH2COO)(PPh3)] revealed volatile products of decomposition (CO2, Me3 Si-) and recombination reactions such as (Me3SiCH2CO)2O, (Me3Si)2O. The mechanism of complexes thermal decomposition is proposed.

Dimeric Silver(I) Complexes with Trimethylphosphine and Aliphatic Perfluorinated Carboxylates

Szłyk E., Łakomska I.

Polish Journal of Chemistry

2002

Vol. 76 / nr 10

1399-1403

Silver(I) complexes with trimethylphosphine and perfluorinated carboxylates of general formula [{Ag(PMe3)2}2(_-OOCR)2], where R = CF3, C2F5, C3F7, C4F9, C7F15, have been prepared and characterized with IR, 1H, 13C, 19F, 31P NMR. Spectral analysis suggests four coordinated Ag(I) with two monodentate trimethylphosphine and bidentate carboxylates forming bridges between silver(I) ions. Thermal decomposition process was studied between 293-973 K in nitrogen. Decomposition proceeds in one exothermic stage corresponding to the elimination of perfluorinated carboxylate and trimethylphosphine. The final product was a mixture of metallic silver and carbon, formed between 473-633 K.

Multinuclear NMR Characterization of Ag(I) Perfluorinated Carboxylates Complexes with Bis(diphenylphosphino)methane

Szłyk E., Goliński A.

Polish Journal of Chemistry

2000

Vol. 74, nr 7

895-901

Ag(I) perfluorinated carboxylate complexes with bis(diphenylphosphino0methane (dppm) of general formula [Ag2(RCOO)2(dppm)], where R=CF3, C3F7, C4F9, C6F13, C9F19 were synthetized and spectroscopically (1H,13C,31P,19F, NMR and IR) characterized. Temperature variable 31P NMR spectra were recorded and 1J(107Ag-31P), ysis of coordination shifts and coupling constants are in favour of dimetric trigonal Ag(I) complexes with bridging carboxylates and dppm in solution. IR spectra suggest the same coordination mode in the solid state.

Spectroscopic and Thermal Studies of Silver(I) Complexes with Aliphatic Carboxylates and Triphenylphosphine

Szłyk E., Łakomska I., Surdykowski A., Goliński A.

Polish Journal of Chemistry

1999

Vol. 73, nr 11

1763-1769

Results of spectral analysis are in favour of Ag(I) trigonal coordination with unidentately bonded triphenylphosphine and bidentate carboxylates, forming bridges between silver(I) ions. Thermal decomposition was studied in 293-973 K range in nitrogen. The multistage decomposition initiates with the detachment of carboxylates and is followed by triphenylphosphine dissociation. The final product is metallic silver, formed between 605-683 K.