Chlorthionitrenkomplexe des Rheniums Die Kristallstruktur von AsPh4[ReCl4(NSCl)2] · CH2Cl2 |
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| Authors: | Ulrich Mü ller,Willi Kafitz,Kurt Dehnicke |
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| Abstract: | Chlorothionitrene Complexes of Rhenium. Crystal Structure of AsPh4[ReCl4(NSCl)2] · CH2Cl2 Rhenium pentachloride reacts in POCl3 solution with (NSCl)3 forming the chlorothionitrene complexes [(Cl3PO)ReCl4(NSCl)] ( I ) and [(Cl3PO)ReCl3(NSCl)2] ( II ). I reacts with AsPh4Cl in CH2Cl2 solution under abstraction of SCl2 and POCl3, yielding AsPh4[ReNCl4], while II forms the complex AsPh4[ReCl4(NSCl)2] · CH2Cl2. The i.r. spectra of the compounds are discussed and assigned. The crystal structure of AsPh4[ReCl4(NSCl)2] · CH2Cl2 was determined and refined with X-ray diffraction data (R = 0.031 for 2785 reflexions). It crystallizes in the space group Pī with two formula units per unit cell; the lattice constants are a = 1119, b = 1144, c = 1473 pm, α = 77.6, β = 70.8 and γ = 71.2°. The two NSCl ligands have cis arrangement with nearly linear Re?N?S groups, with interatomic distances corresponding to double bonds. The Re? Cl bonds are somewhat longer than usual and show no trans-effect; this is possibly due to Cl…?H? C bridges. |
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