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1
Multinuclear NMR and MS Characterization of Silver(I) Perfluorocarboxylates Complexes with 1,4-Bis(diphenylphosphino)butane
Szymańska I., Goliński A., Pazderski L., Szłyk E
Polish Journal of Chemistry
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2007
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Vol. 81, nr 3
299-311
EN
Ag(I) perfluorinated carboxylates complexes with 1,4-bis(diphenylphosphino)butane (dppb) of general formulae [Ag2(dppb)(RCOO)2]n, where R = C2F5, C3F7, C4F9, C6F13, C8F17 have been prepared and characterized by MS, 1H, 13C, 19F, 31P NMR and IR spectroscopy. In the solid state Ag(I) compounds are most likely tetranuclear species bridged by both diphosphines and carboxylates, because MS studies revealed multinuclear metallated species with bridging dppb and carboxylates. Variable temperature (VT) 31P NMR spectra demonstrate that studied complexes form binuclear species bonded by diphosphine with intermolecular diphosphine exchange, in chloroform solution. Thermal studies of Ag(I) compounds revealed three stages decomposition processes (exothermic) resulting in metallic silver formation in the range 713-853 K.
2
Synthesis and Characterization of Ionic Cu(I) Perfluorocarboxylate Compounds with 1,4-Bis(diphenylphosphino)butane
Szymańska I., Pazderski L., Kucharek R., Szłyk E.
Polish Journal of Chemistry
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2005
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Vol. 79 / nr 11
1705-1711
EN
A series of ionic Cu(I) perfluorocarboxylate compounds with 1,4-bis(diphenyl - phosphino)bu tane (dppb) of gen eral formula [Cu(dppb)2](RCOO), where R = C2F5, C3F7, C4F9, C6F13, C8F17, was prepared and characterized with MS, IR and 1H, 13C, 19F, 31P NMR spectroscopy. The studied species contained monomeric, bis-chelated [Cu(dppb)2]+ cations and uncoordi nated RCOO- anions. The Cu(I) coordi nation of the diphosphines resulted in slight high-frequency shifts of the 31P NMR resonances of the equivalent phosphorus atoms.
3
Copper(I) complexes as potential CVD precursors - studies in the liquid state and gas phase
Szymańska I., Kucharek R., Szłyk E.
Materials Science
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2003
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Vol. 21, No. 2
245-250
EN
Cu(I) complexes with trimethyl phosphite and aliphatic perfluorinated carboxylates of the type [Cu2{P(OMe)3}2(m-RCOO)2] where R = CF3, C2F5, C3F7, C6F13, C7F15, C8F17, C9F19 have been prepared as viscous liquids. In the liquid state the spectroscopic results suggest the dimeric structures for complexes, where the metal ions are linked by the bridging carboxylates. This type of bonding was revealed in the gas phase as well. In the MS conditions the most intensive signals were observed for the [Cu2(RCOO)]+ and [Cu2(RCOO)2]+ fragments. Thermal decomposition of complexes proceeds as a multistage process, yielding a Cu2O in the most of cases.
4
Dimeric Silver(I) Complexes with Trimethylphosphine and Aliphatic Perfluorinated Carboxylates
Szłyk E., Łakomska I.
Polish Journal of Chemistry
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2002
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Vol. 76 / nr 10
1399-1403
EN
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.
5
New Polymeric Copper(II) Complexes with Tributy I Phosphite and Perfluorinated Carboxylates
Szłyk E., Szymańska I., Kucharek R., Wrzeszcz G., Rozpłoch F.
Polish Journal of Chemistry
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2001
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Vol. 75, nr 2
215-222
EN
New Cu(II) complexes with tributyl phosphite and aliphatic perfluorinated carboxylates [Cu{P(OBu)3}(ž-OH)(ž-RCOO)]n, where R = CF3, C2F5, C3F7, C6F13, C7F15, were obtained and their spectroscopic (UV-VIS, EPR, MS, IR) and thermal properties were studied. Mass spectra were in favour of the bridging coordination carboxylates and monodentate phosphite and suggest a polymeric structure. EPR spectra and magnetic susceptibility measurements indicate the formation of pentacoordinated Cu(II) in polymeric complexes. Examination of COO absorption bands suggests bridging carboxylates as well as a hydroxo group, whereas tributyl phosphite is monodentately bonded. Thermal decomposition is a multistage process, which in nitrogen and air yields a mixture of Cu2O and Cu2P2O7.
6
New Copper(I) Perfluorinated Carboxylates Complexes with Bis(diphenylphosphine)methane
Szłyk E., Kucharek R., Szymańska I.
Polish Journal of Chemistry
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2001
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Vol. 75, nr 3
337-344
EN
Copper(I) perfluorinated carboxylates complexes with bis(diphenylphosphine)methane (dppm) of general formula [Cu2(ž-dppm)3(RCOO)2] dppm, whereR=C2F5, C4F9, C6F13, C8F17, C9F19, have been prepared and characterized by vibrational, 31P CPMASNMRand 13C CPTOSSB NMR mass spectra in the solid state. 1H, 13C, 19F NMR and variable temperature 31P NMR spectra were measured in solution. Temperature variable 31P NMR spectra revealed at least three dimeric species in equilibrium. IR and mass spectra analyses suggest dimeric complexes with three bridging diphosphines and monodentate carboxylates in the solid state.
7
New Polymeric Copper(II) Complexes with Triphenyl Phosphite and Perfluorinated Carboxylates
Szłyk E., Szymańska I., Wrzeszcz G., Rozpłoch F.
Polish Journal of Chemistry
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2000
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Vol. 74, nr 7
909-918
EN
New Cu(II) complexes with triphenyl phosphite and aliphatic perfluorinated carboxylates [Cu{P(OC6H5)3}(u-OH)(u-RCOO)]n (where R=CF3, C2F5, C3F7, C6F13, C7F15, C8F17, C9F19) were obtainedf and their spectroscopic and thermal properties studied. EPR spectra and magnetic susceptibility measurments indicate the formation of polymeric complexes. Examination of COO absorption bands suggests bridging carboxylates as well as a hydro group, whereas triphenyl phosphite is monodentately bonded. Thermal decomposition is a multistage process, which in nitrogen yields a mixture of Cu, Cu2O and Cu2p2O7 but in air - pure u2P2O7.
8
Multinuclear NMR Characterization of Ag(I) Perfluorinated Carboxylates Complexes with Bis(diphenylphosphino)methane
Szłyk E., Goliński A.
Polish Journal of Chemistry
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2000
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Vol. 74, nr 7
895-901
EN
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.
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