Zinkselenid- und Zinktelluridcluster mit Phenylselenolat- und Phenyltellurolatliganden. Die Kristallstrukturen von [NEt4]2[Zn4Cl4(SePh)6], [NEt4]2[Zn8Cl4Se(SePh)12], [Zn8Se(SePh)14(PnPr3)2], [HPnPr2R]2[Zn8Cl4Te(TePh)12] (R = nPr, Ph) und [Zn10Te4(TePh)12(PR3)2] (R = nPr, Ph)
Abstract
deZnCl2 reagiert mit PhSeSiMe3 bzw. einem Gemisch von PhSeSiMe3/Se(SiMe3)2 in Anwesenheit von NEt4Cl zu den ionischen Komplexen [NEt4]2 · [Zn4Cl4(SePh)6] 1 bzw. [NEt4]2[Zn8Cl4Se(SePh)12] 2. Durch Verwendung von PnPr3 anstatt des quarternären Ammoniumsalzes läßt sich aus Toluol die Verbindung [Zn8Se(SePh)14(PnPr3)2] 3 kristallisieren. Umsetzungen von ZnCl2 mit PhTeSiMe3 und tertiären Phosphanen führen in Aceton zur Bildung der ionischen Verbindungen [HPnPr2R]2[Zn8Cl4Te(TePh)12] (R = nPr 4, Ph 5) und in THF zu den neutralen Clustern [Zn10Te4(TePh)12(PR3)2] (R = nPr 6, Ph 7). Die Strukturen von 1–7 konnten durch Einkristall-Röntgenstrukturanalyse aufgeklärt werden. (1: Raumgruppe P21/n (Nr. 14), Z = 4, a = 1212,4(2) pm, b = 3726,1(8) pm, c = 1379,4(3) pm β = 99,83(3)°; 2 Raumgruppe P21/c (Nr. 14), Z = 4, a = 3848,6(8) pm, b = 1784,9(4) pm, c = 3432,0(7) pm, β = 97,78(3)°; 3: Raumgruppe Pnn2 (Nr. 34), Z = 2 a = 2027,8(4) pm, b = 2162,3(4) pm, c = 1668,5(3) pm; 4: Raumgruppe P21/c (Nr. 14), Z = 4, a = 1899,8(4) pm, b = 2227,0(5) pm, c = 2939,0(6) pm, β = 101,35(3)°; 5: Raumgruppe P21/n (Nr. 14), Z = 4, a = 2230,8(5) pm, b = 1919,9(4) pm, c = 3139,5(6) pm, β = 109,97(4)°; 6: Raumgruppe I41/a (Nr. 88), Z = 4, a = b = 2566,0(4) pm, c = 2130,1(4) pm; 7: Raumgruppe P1¯ (Nr. 2), Z = 2, a = 2068,4(4) pm, b = 2187,8(4) pm, c = 2351,5(5) pm, α = 70,36°, β = 84,62°, γ = 63,63°)
Abstract
enZincselenide- and Zinctellurideclusters with Phenylselenolate- and Phenyltellurolateligands. The Crystal Structures of [NEt4]2[Zn4Cl4(SePh)6], [NEt4]2[Zn8Cl4Se(SePh)12], [Zn8Se(SePh)14(PnPr3)2], [HPnPr2R]2[Zn8Cl4Te(TePh)12] (R = nPr, Ph), and [Zn10Te4(TePh)12(PR3)2] (R = nPr, Ph)
In the prescence of NEt4Cl ZnCl2 reacts with PhSeSiMe3 or a mixture of PhSeSiMe3/Se(SiMe3)2 to form the ionic complexes [NEt4]2[Zn4Cl4(SePh)6] 1 or [NEt4]2[Zn8Cl4Se(SePh)12] 2 respectively. The use of PnPr3 instead of the quarternary ammonia salt leads in toluene to the formation of crystalline [Zn8Se(SePh)14(PnPr3)2] 3. Reactions of ZnCl2 with PhTeSiMe3 and tertiary phosphines result in acetone in crystallisation of the ionic clusters [HPnPr2R]2[Zn8Cl4Te(TePh)12] (R = nPr 4, Ph 5) and in THF of the uncharged [Zn10Te4(TePh)12(PR3)2] (R = nPr 6, Ph 7). The structures of 1–7 were obtained by X-ray single crystal structure. (1: space group P21/n (No. 14), Z = 4, a = 1212,4(2) pm, b = 3726,1(8) pm, c = 1379,4(3) pm β = 99,83(3)°; 2 space group P21/c (Nr. 14), Z = 4, a = 3848,6(8) pm, b = 1784,9(4) pm, c = 3432,0(7) pm, β = 97,78(3)°; 3: space group Pnn2 (No. 34), Z = 2, a = 2027,8(4) pm, b = 2162,3(4) pm, c = 1668,5(3) pm; 4: space group P21/c (No. 14), Z = 4, a = 1899,8(4) pm, b = 2227,0(5) pm, c = 2939,0(6) pm, β = 101,35(3)°; 5: space group space group P21/n (No. 14), Z = 4, a = 2231,0(5) pm, b = 1919,9(4) pm, c = 3139,5(6) pm, β = 109,97(4)°; 6: space group I41/a (No. 88), Z = 4, a = b = 2566,0(4) pm, c = 2130,1(4) pm; 7: space group P1¯ (No. 2), Z = 2, a = 2068,4(4) pm, b = 2187,8(4) pm, c = 2351,5(5) pm, α = 70,36°, β = 84,62°, γ( = 63,63°)
