Technetium and rhenium pentacarbonyl perchlorates: Structure and reactivity

Miroslavov, A. E.; Gurziy, V.V.; Tyupina, M. Yu.; Лумпов, А. А.; Sidorenko, G. V.; Polotskii, Yu.S.; Suglobov, D.N.

doi:10.1016/j.jorganchem.2013.07.019

Cited by 14 publications

(13 citation statements)

References 10 publications

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“…These compounds were isolated and characterized in our previous study. 10 We also found previously that the perchlorate ligand in [Tc(ClO 4 )-(CO) 5 ] could be readily substituted by isocyanide ligands. 3 , where TBI is tert-butyl isocyanide).…”

Section: ■ Results and Discussionsupporting

confidence: 64%

Technetium and Rhenium Pentacarbonyl Complexes with C₂ and C₁₁ ω-Isocyanocarboxylic Acid Esters

et al. 2014

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Technetium(I) and rhenium(I) pentacarbonyl complexes with ethyl 2-isocyanoacetate and methyl 11-isocyanoundecanoate, [M(CO)5(CNCH2COOEt)]ClO4 (M = Tc (1) and Re (2)) and [M(CO)5(CN(CH2)10COOMe)]ClO4 (M = Tc (3) and Re (4)), were prepared and characterized by IR, (1)H NMR, and (13)C{(1)H} NMR spectroscopy. The crystal structures of 1 and 2 were determined using single-crystal X-ray diffraction. The kinetics of thermal decarbonylation of technetium complexes 1 and 3 in ethylene glycol was studied by IR spectroscopy. The rate constants and activation parameters of this reaction were determined and compared with those for [Tc(CO)6](+). It was found that rhenium complexes 2 and 4 were stable with respect to thermal decarbonylation. Histidine challenge reaction of complexes 1 and 2 in phosphate buffer was examined by IR spectroscopy. In the presence of histidine, the rhenium pentacarbonyl isocyanide complex partially decomposes to form an unidentified yellow precipitate. Technetium analogue 1 is more stable under these conditions.

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Section: ■ Results and Discussionsupporting

confidence: 64%

Technetium and Rhenium Pentacarbonyl Complexes with C₂ and C₁₁ ω-Isocyanocarboxylic Acid Esters

et al. 2014

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“…For this purpose, [ 99 TcBr(CO) 5 ] was treated with AgClO 4 in dichloromethane at room temperature (See SI). As determined by IR spectroscopy, [ 99 TcBr(CO) 5 ] was quantitatively converted to [ 99 Tc(ClO 4 )(CO) 5 ] [14] . The IR spectrum of [ 99 Tc(ClO 4 )(CO) 5 ] in CH 2 Cl 2 had two characteristic bands at 2074.3 (s) and 2016.4 (m) cm −1 (Figure S1).…”

Section: Resultsmentioning

confidence: 96%

“…For this purpose, [ 99 TcBr(CO) 5 ] was treated with AgClO 4 in dichloromethane at room temperature ]. [14] The IR spectrum of [ 99 Tc(ClO 4 )(CO) 5 ] in CH 2 Cl 2 had two characteristic bands at 2074.3 (s) and 2016.4 (m) cm À 1 (Figure S1). Then carbon monoxide was bubbled through a solution of [ 99 Tc(ClO 4 )(CO) 5 ] thus obtained.…”

Section: Resultsmentioning

confidence: 99%

Synthesis of [⁹⁹Tc(CO)₆]⁺ Cation under Ambient Conditions

et al. 2022

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“…Concomitantly, the donor strength of the P atom decreases due to inductive effects, which, in turn, leads to an increase in the CO vibration frequencies (cf. frequencies of the corresponding bands in the spectra of technetium pentacarbonyl complexes with anionic ligands) [12,16]. At acid concentrations above 3 mol/mol, no further shift of the carbonyl band was observed.…”

Section: Behavior Of the Pentacarbonyl Phosphine Complexes In Aqueous Solutionsmentioning

confidence: 93%

“…For this purpose, we used perchlorate and triflate anions as the readily leaving ligands. Technetium and rhenium pentacarbonyl perchlorates were obtained as described in our previous work [16]. [10].…”

Section: Synthesismentioning

confidence: 99%

Water-soluble carbonyl complexes of 99Tc(I) and Re(I) with adamantane-cage aminophosphines PTA and CAP

Miroslavov

Britvin

Braband

et al. 2019

Journal of Organometallic Chemistry

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Pentacarbonyl complexes of 99Tc and Re [M(CAP)(CO)5]X and [M(PTA)(CO)5]X (M = 99Tc or Re and X = ClO4− or OTf-) with aminophosphine ligands 1,4,7-triaza-9-phosphatricyclo[5.3.214,9]tridecane (CAP) and 1,3,5-triaza-7-phosphaadamantane (PTA) were prepared for the first time by the reaction of [MX(CO)5] (M = 99Tc or Re, X = ClO4− or OTf-) with CAP and PTA in CH2Cl2 at room temperature. The reaction of [TcCl(CO)5] with CAP in refluxing CH2Cl2 yields the tricarbonyl complex [99TcCl(CAP)2(CO)3]. Treatment of [Re(H2O)3(CO)3]Cl with CAP in aqueous solution at 40-50°Cgives the rhenium analog [ReCl(CAP)2(CO)3]. Both penta-and tricarbonyl phosphine complexes were characterized by spectroscopic methods (IR, NMR, MS) and single crystal X-ray diffraction. The [M(PTA)(CO)5]X complexes are soluble in aqueous solutions, whereas their CAP analogs are not. The CAP complexes become water-soluble after acidification with dilute acids. As the pH of their aqueous solutions increases, they start to slowly degrade at pH 8 and completely decompose at pH 14. In acidic media, the pentacarbonyl complexes undergo stepwise protonation and are stable indefinitely.

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Technetium and rhenium pentacarbonyl perchlorates: Structure and reactivity

Cited by 14 publications

References 10 publications

Technetium and Rhenium Pentacarbonyl Complexes with C₂ and C₁₁ ω-Isocyanocarboxylic Acid Esters

Technetium and Rhenium Pentacarbonyl Complexes with C₂ and C₁₁ ω-Isocyanocarboxylic Acid Esters

Synthesis of [⁹⁹Tc(CO)₆]⁺ Cation under Ambient Conditions

Water-soluble carbonyl complexes of 99Tc(I) and Re(I) with adamantane-cage aminophosphines PTA and CAP

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Technetium and rhenium pentacarbonyl perchlorates: Structure and reactivity

Cited by 14 publications

References 10 publications

Technetium and Rhenium Pentacarbonyl Complexes with C2 and C11 ω-Isocyanocarboxylic Acid Esters

Technetium and Rhenium Pentacarbonyl Complexes with C2 and C11 ω-Isocyanocarboxylic Acid Esters

Synthesis of [99Tc(CO)6]+ Cation under Ambient Conditions

Water-soluble carbonyl complexes of 99Tc(I) and Re(I) with adamantane-cage aminophosphines PTA and CAP

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Technetium and Rhenium Pentacarbonyl Complexes with C₂ and C₁₁ ω-Isocyanocarboxylic Acid Esters

Technetium and Rhenium Pentacarbonyl Complexes with C₂ and C₁₁ ω-Isocyanocarboxylic Acid Esters

Synthesis of [⁹⁹Tc(CO)₆]⁺ Cation under Ambient Conditions