The vanadium(II) derivatives [V-2(mu-Cl)(3)(THF)(6)](2)[M(2)Cl(6)] (M = Mn, Fe) have been prepared by reduction of VCl3(THF)(3) with manganese or iron metal powders in THF and structurally characterized for M = Mn. [V-2(mu-Cl)(3)(THF)(6)](2)[Mn2Cl6] crystallizes in the triclinic space group P (1) over bar (No. 2) with a = 10.867(6), b = 11.626(8), c = 15.486(6) Angstrom, alpha = 75.70(4), beta = 71.25(4), gamma = 80.29(5)degrees, V = 1787(2) Angstrom(3), Z = 1. The structure contains discrete [V-2(mu-Cl)(3)(THF)(6)](+) cations and [Mn2Cl6](2-) anions, the anion consisting of two MnCl4 tetrahedra sharing an edge. By treatment of VCl3(THF)(3) with DME the new vanadium(III) coordination compound VCl3(DME)(THF) has been obtained which crystallizes in the space group Pnma (No. 62) with unit cell dimensions a = 14.193(8), b = 11.99(1), c = 7.92(1) Angstrom, V = 1347(2) Angstrom(3), Z = 4. VCl3(DME)(THF) shows a fac-stereochemistry of the ligands in a distorted octahedral coordination around the vanadium atom. The same compound has been obtained by reaction of VCl3(DME)(1.5) with a stoicheiometric amount of THF in toluene.
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