Reactions of [ReOCl3(PPh3)2] with 4‐Fluoroaniline

Scholtysik, Clemens; Jungfer, Maximilian Roca; Hagenbach, Adelheid; Abram, Ulrich

doi:10.1002/zaac.201800240

Cited by 7 publications

(28 citation statements)

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“…Similar results have been found in a series of related complexes before . The corresponding Re1–O10 (1.688(5)‐1.699(5) Å) and Re1–N10 bonds (1.720(3)‐1.728(3) Å) are in the usual ranges and the imido ligands are linear .…”

Section: Resultssupporting

confidence: 86%

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Rhenium(V) Complexes with Selenolato‐ and Tellurolato‐Substituted Schiff Bases – Released PPh₃as a Facile Reductant

et al. 2019

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The salicylidene Schiff bases of bis(2-aminophenyl)diselenide and -ditelluride react with [ReOCl 3 (PPh 3 ) 2 ] or the arylimidorhenium(V) compounds [Re(NPhR)Cl 3 (PPh 3 ) 2 ] (R = H, F, CF 3 ) with formation of rhenium(V) complexes with tridentate {O,N,Se/Te} chalcogenolato ligands. The ligands adopt a facial coordination mode with the oxygen donors trans to the multiply bonded O 2or NPhR 2ligands. The reduction of the dichalcogenides and the formation of the chalcogenolato ligands oc-[a]

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Section: Resultssupporting

confidence: 86%

“…(NBu 4 )[ReOCl 4 ], [ReOCl 3 (PPh 3 ) 2 ], [Re(NPh)Cl 3 (PPh 3 ) 2 ], [Re(NPhF)Cl 3 (PPh 3 ) 2 ], bis(2‐aminophenyl)diselenide and bis(2‐aminophenyl)ditelluride were prepared according to literature procedures . All other chemicals were reagent grade and used as received.…”

Section: Methodsmentioning

confidence: 99%

Rhenium(V) Complexes with Selenolato‐ and Tellurolato‐Substituted Schiff Bases – Released PPh₃as a Facile Reductant

et al. 2019

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“…17,18 Recently, we reported the synthesis of the fluorinated phenylimido complex [Re(NPhF)Cl 3 (PPh 3 ) 2 ]. 19 This compound shows a solubility considerably higher than that of [Re(NPh)Cl 3 (PPh 3 ) 2 ] and might be a good candidate for controlled ligand exchange reactions. In this study, we extend the chemistry of fluorinated phenylimido ligands to technetium and describe the syntheses, structures, and spectroscopic behavior of some {M(NPhF)} 3+ (M = Re or Tc) complexes with fluorinated β-diketonato ligands.…”

Section: ■ Introductionmentioning

confidence: 99%

“…1 H NMR (CDCl 3 ): δ 6.34 (s, 1H, CH), 3.18 (dd, 2H, CH 2 ), 1.62 (dd, 2H, CH 2 ), 1.41 (dd, 2H, CH 2 ), 0.99 (t, 3H, CH 3 ). 19 F NMR (CDCl 3 ): δ −72.3 (s, 3F, CF 3 ), −73.7 (s, 3F, CF 3 ). 13 C NMR (CDCl 3 ): δ 182.8 (d, J = 37 Hz, 1C, CO), 179.3 (d, J = 37 Hz, 1C, CO), 114.2 (q, J = 280 Hz, 1C, CF 3 ), 113.7 (q, J = 280 Hz, 1C, CF 3 ), 84.5 (s, 1C, CH), 60 (s, 4C, CH 2 ), 24.4 (s, 4C, CH 2 ), 20 (s, 4C, CH 2 ), 13.8 (s, [Tc(NPhCF 3 )Cl 3 (PPh 3 ) 2 ].…”

Section: ■ Introductionmentioning

confidence: 99%

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Complexes of Technetium(V) and Rhenium(V) with β-Diketonates

et al. 2019

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Reactions of (NBu4)[MOCl4] complexes (M = Tc or Re) with an excess of hexafluoroacetylacetone (Hhfac) give products with a composition of (NBu4)[MOCl3(hfac)] as bright yellow (Tc) or red (Re) solids. The products are stable as solids but rapidly decompose in solution. A number of related phenylimidorhenium(V) complexes were synthesized starting from [Re(NPhF)Cl3(PPh3)2], where (NPhF)2– is a para-fluorinated phenylimido ligand. Products with compositions of [Re(NPhF)Cl2(PPh3)(acac)], [Re(NPhF)Cl2(PPh3)(hfac)], [Re(NPhF)Cl2(PPh3)(tfac)], [Re(NPhF)Cl2(PPh3)(naphtfac)], and [Re(NPhF)Cl2(PPh3)(tbutfac)] (Hacac = acetylacetone, Htfac = trifluoroacetylacetone, Hnaphtfac = naphthoyltrifluoroacetylmethane, and Htbutfac = tert-butyroyltrifluoroacetylmethane) were isolated from reactions of the quite soluble [Re(NPhF)Cl3(PPh3)2] with the corresponding β-diketones and studied spectroscopically and by X-ray diffraction. The β-diketonates are coordinated in a meridional arrangement with the phenylimide. The formation of two isomers was detected for nonsymmetric β-diketones with a preference for the “equatorial” position for the more bulky substituents. Products with more than one chelating ligand were not obtained. The technetium complexes [Tc(NPhX)Cl3(PPh3)2] (X = p-F or p-CF3) were prepared from reactions of pertechnetate, PPh3, HCl, and substituted arylacetylhydrazines and isolated as green solids. They are sufficiently stable as solid but rapidly decompose in moist solvents upon hydrolysis of the Tc–N bonds. From reactions of [Tc(NPh)Cl3(PPh3)2] or [Tc(NPhF)Cl3(PPh3)2] in dry solvents, the complexes [Tc(NPh)Cl2(PPh3)(hfac)] and [Tc(NPhF)Cl2(PPh3)(hfac)] were prepared and isolated in crystalline form. An X-ray diffraction study shows that fluorination of the para position of the phenylimido ligand results in a slight lengthening of all bonds in the coordination sphere of technetium.

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Reactivity of [ReOCl₃(PPh₃)₂] Towards Substituted Anilines

Cvetković,

Theiner,

Wolff

et al. 2024

Zeitschrift anorg allge chemie

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The reactivity of [ReOCl3(PPh3)2] towards o‐toluidine, m‐toluidine, o‐fluoroaniline, m‐fluoroaniline, p‐bromoaniline, p‐chloroaniline and p‐anisidine was examined and novel rhenium(V) imido complexes [Re(NC6H4R)Cl3(PPh3)2] (R = o‐Me, m‐Me, o‐F, m‐F, p‐Cl, p‐Br, p‐OMe) were obtained. The resulting products were characterized by elemental analysis, electrospray ionization high‐resolution mass spectrometry (ESI‐HRMS), 1H, 13C{1H}, 19F{1H} and 31P{1H} NMR, FT‐IR spectroscopy, and X‐ray crystallography. For m‐toluidine, m‐fluroaniline and p‐chloroaniline, rhenium(V) imido‐amino mononuclear [Re(NC6H4R)Cl3(H2NC6H4R)(PPh3)] (R = m‐F, p‐Cl) complexes and binuclear [{Re(m‐NC6H4Me)Cl2(m‐H2NC6H4Me)(PPh3)}2O] complex were isolated as side products and characterized by X‐ray crystallography. All six‐coordinate rhenium(V) complexes display distorted octahedral coordination geometry.

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Reactions of [ReOCl₃(PPh₃)₂] with 4‐Fluoroaniline

Cited by 7 publications

References 20 publications

Rhenium(V) Complexes with Selenolato‐ and Tellurolato‐Substituted Schiff Bases – Released PPh₃as a Facile Reductant

Rhenium(V) Complexes with Selenolato‐ and Tellurolato‐Substituted Schiff Bases – Released PPh₃as a Facile Reductant

Complexes of Technetium(V) and Rhenium(V) with β-Diketonates

Reactivity of [ReOCl₃(PPh₃)₂] Towards Substituted Anilines

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Reactions of [ReOCl3(PPh3)2] with 4‐Fluoroaniline

Cited by 7 publications

References 20 publications

Rhenium(V) Complexes with Selenolato‐ and Tellurolato‐Substituted Schiff Bases – Released PPh3as a Facile Reductant

Rhenium(V) Complexes with Selenolato‐ and Tellurolato‐Substituted Schiff Bases – Released PPh3as a Facile Reductant

Complexes of Technetium(V) and Rhenium(V) with β-Diketonates

Reactivity of [ReOCl3(PPh3)2] Towards Substituted Anilines

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Reactions of [ReOCl₃(PPh₃)₂] with 4‐Fluoroaniline

Rhenium(V) Complexes with Selenolato‐ and Tellurolato‐Substituted Schiff Bases – Released PPh₃as a Facile Reductant

Rhenium(V) Complexes with Selenolato‐ and Tellurolato‐Substituted Schiff Bases – Released PPh₃as a Facile Reductant

Reactivity of [ReOCl₃(PPh₃)₂] Towards Substituted Anilines