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Syntheses and reactivity of sulphur rich Re(III) and Tc(III) complexes containing trithioperoxybenzoate, dithiobenzoate and dithiocarbamate ligands (Articolo in rivista)

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Syntheses and reactivity of sulphur rich Re(III) and Tc(III) complexes containing trithioperoxybenzoate, dithiobenzoate and dithiocarbamate ligands (Articolo in rivista) (literal)

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Lepareur N.; Mévellec F.; Noiret N.; Refosco F.; Tisato F.; Porchia M.; Bandoli G. (2005)
Syntheses and reactivity of sulphur rich Re(III) and Tc(III) complexes containing trithioperoxybenzoate, dithiobenzoate and dithiocarbamate ligands
in Dalton transactions (2003. Print)
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Lepareur N.; Mévellec F.; Noiret N.; Refosco F.; Tisato F.; Porchia M.; Bandoli G. (literal)

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1-3 Ecole Nationale Supérieure de Chimie de Rennes, UMR CNRS 6052, Synthèses et Activations de Biomolécules, Institut de Chimie de Rennes, Rennes, France 4-6 ICIS-CNR, Corso S. Uniti, 4 35127 Padova, Italy 7 Dipartimento di Scienze Farmaceutiche, Università di Padova, Via Marzolo 5, 35131 Padova, Italy (literal)

Titolo

Syntheses and reactivity of sulphur rich Re(III) and Tc(III) complexes containing trithioperoxybenzoate, dithiobenzoate and dithiocarbamate ligands (literal)

Abstract

Reduction-substitution reactions of [M(O)Cl4]- (M = Re, 99Tc) precursors with an excess of substituted dithiobenzoate ligands (R-PhCS2)- in dichloromethane/methanol mixtures afford a series of six-coordinated neutral mixed-ligand complexes of the type MIII(R-PhCS3)2(R-PhCS2), (M = Re; Re1-9; M = 99Tc; Tc1-9). The coordination sphere is entirely filled by sulphur donor atoms, and the complexes adopt a distorted trigonal prismatic arrangement, as assessed by the X-ray crystal structure analysis of Re(4-Me-PhCS3)2(4-Me-PhCS2), Re2. These compounds show sharp proton and carbon NMR profiles, in agreement with the diamagnetism typical of low spin d4 trigonal prismatic configurations. The red-ox processes involve reduction of the metal from Re(V) to Re(III) and oxidation of dithiobenzoate to trithioperoxybenzoate. M2-9 complexes contain a substitution-inert [M(R-PhCS3)2]+ moiety including the metal and two trithioperoxybenzoate fragments, while the third dithiobenzoate ligand is labile. The latter is efficiently replaced by reaction with better nucleophiles such as diethyldithiocarbamate giving a further class of mixed ligand complexes of the type MIII(R-PhCS3)2(Et2NCS2), (M = Re; Re10-18; M = 99Tc; Tc10-18), which retain the trigonal prismatic arrangement, as determined by the X-ray analyses of the representative compounds Re(PhCS3)2(Et2NCS2), Re10 and 99Tc(PhCS3)2(Et2NCS2), Tc10. (literal)

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