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The title compounds were obtained from NiS + PPh 4 Cl + HCl in dichloromethane, from NiCl 2  and PPh 4 Cl and from NiCl 2  + Na 2 S + 15-crown-5 in acetonitrile or CH 2 Cl 2 , respectively. Their crystal structures were determined by X-ray diffraction. (PPh 4 ) 2 [NiCl 4 ]: monoclinic, space group C 2/c, Z = 4, a = 1094.9(3), b = 1946.1(4), c = 2033.5(5) pm, β = 91.48(3)°; R = 0.07 for 2895 unique observed reflexions. [Na-15-crown-5] 2 [NiCl 4 ]: triclinic, space group P1̄, Z = 2, a = 987.6(1), b = 998.0(1), c = 1779.9(2) pm, α = 104.17(1), β = 95.43(1), γ = 109.95(1)°; R = 0.090 for 4155 unique observed reflexions. In both cases, the [NiCl 4 ] 2-  ions have distorted tetrahedral structures. With PPh 4  +  as the cation the distortion corresponds to a twisted tetrahedron which fulfils the point symmetry D 2 , the deviation from a flattened D 2d -tetrahedron being small. In (PPh 4 ) 2 [NiCl 4 ] cations and anions alternate in layers parallel to (001). In [Na-15-crown-5] 2 [NiCl 4 ] two of the Cl atoms of the anion are coordinated to sodium ions; one of the crown ether molecules shows positional disorder.

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Kristallstrukturen der Tetrachloroniccolate (PPh 4 ) 2 [NiCl 4 ] und [Na-15-Krone-5] 2 [NiCl 4 ] / Crystal Structures of the Tetrachloroniccolates (PPh 4 ) 2 [NiCl 4 ] and [Na- 15-Crown-5] 2 [NiCl 4 ]