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Reaction of nickel(II) chloride with disodium ο-xylenediselenolate in methanol yields the trinuclear mixed selenide-selenolate complex anion [Ni 3 Se(ο-C 6 H 4 {CH 2 Se} 2 ) 3 ] 2-  (3) which was isolated both as tetramethylammonium and mixed sodium/tetraethylammonium salt of formula [Me 4 N] 2 [Ni 3 Se(ο-C 6 H 4 {CH 2 Se} 2 ) 3 ] · MeOH (1) and [Et 4 N] 3 Na[Ni 3 Se-(ο-C 6 H 4 {CH 2 Se} 2 ) 3 ] 2-  · 3MeOH · 3H 2 O (2), respectively. Crystals of 1 are triclinic, space group P1̄, a = 9.065(2), b = 13.281(3); c = 18.019(4) Å , α = 92.81(2), β = 97.55(2), γ = 105.09(2)° and Z = 2. 2 crystallizes in the rhom bohedral space group R3c with a = 20.305(5), c = 41.709(9) Å and Z = 6. The structures were refined to R = 0.0705 (1) and 0.0794 (2), respectively. Both compounds contain the complex anion [Ni 3 Se- (ο-C 6 H 4 {CH 2 Se} 2 ) 3 ] 2-  (3), which possesses the same principal structural features as the corresponding thiolato derivatives. Reaction of nickel(II) chloride with sodium iso-propane selenolate in methanol leads to the cyclic tetranuclear complex [Ni 4 (Se i C 3 H 7 ) 8 ] (4), which crystallizes in the monoclinic space group P2/n with a = 13.161(3), b = 10.464(2), c = 14.603(2) Å , β = 94.42(1)° and Z = 2. The structure refinement converged to R = 0.0541. 4 is isostructural with the corresponding thiolato compound. The introduction of selenium instead of sulfur ligands reduces the midpoint potential of the reversible metal-centered oxidation from +595 to +285 mV.

zeitschrift für naturforschung b

[Ni 3 Se(o-C 6 H 4 {CH 2 Se} 2 ) 3 ] 2-  und [Ni 4 (Se i C 3 H 7 ) 8 ], die ersten höherkernigen NickeI(II)-Komplexe mit vollständiger Selen-Ligandensphäre [Ni 3 Se(o-C 6 H 4 {CH 2 Se} 2 ) 3 ] 2-  and [Ni 4 (Se i C 3 H 7 ) 8 ], the First Polynuclear Nickel(II) Complexes with Complete Selenium Ligand Spheres