X-Ray molecular structures of [Zn(C3Se5)2]2– and [Zn(CSe4)2]2– anion complexes
Abstract
The salts [PPh4]2[Zn(C3Se5)2](1) and [PPh4]2[Zn(CSe4)2](2) were isolated from a solution of carbon diselenide with sodium metal in the presence of zinc(II) chloride and [PPh4]Br in dimethyl sulphoxide or in MeOCH2CH2OCH2CH2OMe. Single-crystal X-ray structure analyses were performed for these complexes: (1)·MeCN, triclinic, space group P, a= 17.402(3), b= 19.353(4), c= 9.774(4)Å, α= 99.59(3), β= 98.37(3), γ= 65.51(2)°, and Z= 2; (2) monoclinic, space group P21/n, a= 21.586(2), b= 24.136(2), c= 10.208 4(7)Å, β= 104.87(7)°, and Z= 4. The structure refinements converged to R= 0.060 and 0.072 for (1) and (2), respectively. Both complexes assume a tetrahedral geometry around the metal atom, the ligands being almost planar. Electronic absorption and 77Se n.m.r. spectra of the complexes were measured.