Synthesis and structural characterization of dialkyldithiocarbamato complexes of niobium

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Juan Fernández-Baeza, Félix A. Jalón, Antonio Otero, Ma Esther Rodrigo-Blanco and Michel Etienne


Abstract

The reaction of alkyne-containing niobium(III) complexes [NbCl3(dme)(RC[triple bond, length half m-dash]CR′)] (dme = 1,2-dimethoxyethane) with the appropriate Na(S2CNR″2) reagents, in a 1∶3 molar ratio, afforded the corresponding dialkyldithiocarbamato complexes [Nb(RC[triple bond, length half m-dash]CR′)(S2CNR″2)3] (R = R′ = Ph, R″ = Me 1; R = R′ = Ph, R″ = Et 2; R = R′ = R″ = Me 3; R = R′ = Me, R″ = Et 4; R = R′ = Et, R″ = Me 5; R = R′ = R″ = Et 6; R = R′ = SiMe3, R″ = Me 7; R = R′ = SiMe3, R″ = Et 8; R = Ph, R′ = Me, R″ = Me 9). The same complexes were also prepared from the reaction of the appropriate [NbCl3(bpzm)(RC[triple bond, length half m-dash]CR′)] [bpzm = bis(pyrazol-1-yl)methane] complexes with the corresponding sodium dialkyldithiocarbamates. All complexes were spectroscopically characterized and the dynamic behaviour of some of them was studied by variable-temperature NMR techniques. The molecular structure of complex 9 was also established.


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