Abstract
Abstract S-alkylated derivatives of [Ni(DDDT)2]2- (DDDT2 2- = 5,6-dihydro-1,4-dithiin-2,3-dithiolate) and [Ni(PDDT)2]2- (PDDT2 2- = 1,3-propanediyldithioethylene-1,2-dithiolate) were synthesized and characterized. The syntheses were carried out by alkylation (CH3I) of the dianions under inert atmospheric conditions. Crystals of [Ni(CH3-S4C4H4)2] were grown at 25°C from saturated CH2Cl2. The structure was determined by X-ray crystallography. The crystals were monoclinic, space group P21/c, a = 7.1860(20) A, b = 10.3930(9) A, c = 11.831(6) A, β = 107.12(4)°, V = 844.4(5) A3, and Z = 2. Variable temperature 1H-NMR studies revealed evidence of dynamic behavior in solution. Cyclic voltammetry showed the presence of an electrochemically reversible (chemically irreversible) reduction product.
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