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The reaction of CuCl2-2H2O or NiCl2.6H2O with K2(C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu(C5H6S4)2]- or [Ni(C5H6S4)2]- as the tetrabutylammonium salt. Both complexes show characteristic IR and UV-Vis absorptions of transition metal dithiolenes. Cyclic voltammograms contain two waves indicating a two step electrochemical procedure [M(C5H6S4)2]0 = [M(C5H6S4)2]1-= [M(C5H6S4)2]2-. Single crystal structure study has been carried out on the nickel complex. Crystal of [Bu4N][Ni(C5H6S4)2] belongs to monoclinic space group P21/c with a=17.576(5), 6=10.883(2), c=17.773(4) A,B=91.07(2)0, Z=4, and o(calcd.)=1.348 g/cm3. Final result is R=0.059 for 2959 reflections. The NiS4 core exhibits square planar coordination with average Ni-S bond length of 2.134(5) A. There are not anion pairs in crystal. The anions stack along a and c axes while the cations intercalate in them. The nearest S-S contact is 4.429 A. The solid powder ESR s
The reaction of CuCl2-2H2O or NiCl2.6H2O with K2 (C5H6S4) [potassium salt of 6,7-dihydro-5H-1,4-dithiepin-2,3-dithiolate] under nitrogen atmosphere resulted in the isolation of [Cu Both complexes show characteristic IR and UV-Vis absorptions of transition metal dithiolenes. Cyclic voltammograms contain two waves indicating a two step electrochemical procedure [M (C5H6S4) 2] - or [Ni (C5H6S4) 2] - as the tetrabutylammonium salt. Crystal structure of [Bu4N] [Ni (C5H6S4) 2] belongs to the following group: [M (C5H6S4) 2] 1- = [M to monoclinic space group P21 / c with a = 17.576 (5), 6 = 10.883 (2), c = 17.773 (4) A, B = 91.07 (2) 0, Z = 4, and o (calcd. g / cm3. Final result is R = 0.059 for 2959 reflections. The NiS4 core exhibits square planar coordination with average Ni-S bond length of 2.134 (A) A. There are not anion pairs in crystal. The anions stack along a and c axes while the cations intercalate in them. The nearest SS contact is 4.429 A. The solid powder ESR s