Attempts to optimise the synthesis of a new class of nickel(ll) dithiolene complexes starting from 1,3-dialkylimidazolidine-2-thione-4,5- dione (1) and Lawesson's reagent (2) have afforded a new and easy one step synthesis of phosphonodithioate nickel(II) complexes. This consists of the direct reaction between NiCl2 and Lawesson's reagent in the appropriate alcohol R'OH (R=Me, Et, i-Pr, Bu, Bz) as solvent, to give the bis-[O-alkyl/aryl-(4-methoxyphenyl)phosphonodithioato] nickel(II) complexes (5a-e) with high yields (64-91%). Among them trans-bis-[O-ethyl-(4-methoxyphenyl) phosphonodithioato] nickel(II) (5b) was characterised by means of X-ray diffraction measurements on a single crystal. The compound crystallises in the triclinic, Pi space group with a= 6.4840(7), b = 7.6032(9), c= 13.055(2) Angstrom, alpha = 99.481(9), beta = 99.43(1), gamma = 104.487(9)degrees and Z = 1. The compound is centrosymmetric and exhibits discrete monomeric units with the ligand acting as S,S-bidentate. To explain the reactivity of Lawesson's reagent, the formation of 4-methoxyphenyldithiophospborane (6) as intermediate has been suggested. The reaction was also tested for Pd(II) and Pt(II), but in these cases the yields were not as satisfactory as for Ni(II).
New Perspectives in Phosphonodithioate Coordination Chemistry. Synthesis and X-ray Crystal Structure of Trans-bis-[O-ethyl(4-methoxyphenyl)phosphonodithioato] nickel(II) / M., Arca; Cornia, Andrea; F. A., Devillanova; FABRETTI COSTANTINO, Antonio; F., Isaia; V., Lippolis; G., Verani. - In: INORGANICA CHIMICA ACTA. - ISSN 0020-1693. - STAMPA. - 262:(1997), pp. 81-84.
New Perspectives in Phosphonodithioate Coordination Chemistry. Synthesis and X-ray Crystal Structure of Trans-bis-[O-ethyl(4-methoxyphenyl)phosphonodithioato] nickel(II)
CORNIA, Andrea;FABRETTI COSTANTINO, Antonio;
1997
Abstract
Attempts to optimise the synthesis of a new class of nickel(ll) dithiolene complexes starting from 1,3-dialkylimidazolidine-2-thione-4,5- dione (1) and Lawesson's reagent (2) have afforded a new and easy one step synthesis of phosphonodithioate nickel(II) complexes. This consists of the direct reaction between NiCl2 and Lawesson's reagent in the appropriate alcohol R'OH (R=Me, Et, i-Pr, Bu, Bz) as solvent, to give the bis-[O-alkyl/aryl-(4-methoxyphenyl)phosphonodithioato] nickel(II) complexes (5a-e) with high yields (64-91%). Among them trans-bis-[O-ethyl-(4-methoxyphenyl) phosphonodithioato] nickel(II) (5b) was characterised by means of X-ray diffraction measurements on a single crystal. The compound crystallises in the triclinic, Pi space group with a= 6.4840(7), b = 7.6032(9), c= 13.055(2) Angstrom, alpha = 99.481(9), beta = 99.43(1), gamma = 104.487(9)degrees and Z = 1. The compound is centrosymmetric and exhibits discrete monomeric units with the ligand acting as S,S-bidentate. To explain the reactivity of Lawesson's reagent, the formation of 4-methoxyphenyldithiophospborane (6) as intermediate has been suggested. The reaction was also tested for Pd(II) and Pt(II), but in these cases the yields were not as satisfactory as for Ni(II).Pubblicazioni consigliate
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