Five new Ni(dmit)2 anion radical salts, [Me3Te][Ni(dmit)2]2 (1), [Me3Te][Ni(dmit)2]3·(CH3)2C(O) (2), α-[MOT][Ni(dmit)2]2 (3), β-[MOT][Ni(dmit)2]2 (4), and γ-[MOT][Ni(dmit)2]2 (5) (dmit = 1,3-dithiole-2-thione-4,5-dithiolate; MOT = 1-oxa-4-methyl-4-telluracyclohexane) have been prepared by galvanostatic electrolysis. X-Ray crystal structure analyses show that all the salts are characterized by short Te⋯S contacts (3.41–3.85 Å) between the anions and cations. Each salt shows unique molecular packing of the Ni(dmit)2 units. The electronic structures are strongly dependent on these unique molecular arrangements. Among them, 1 and 3 show metallic behavior (down to 60 and 160 K, respectively) and the resistivity of 4 is almost independent of temperature, increasing moderately below 40 K.
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