Addukte des Oxo-tetrachloro-niobat(V)-Ions Bildung,Schwingungsspektren und Kristallstrukturen von PPh4[NbOCl4(OH2)] und (PPh4)2[NbOCl4(O2PCl2)] · 2 CH2Cl2 |
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Authors: | Paul Klingelhfer Ulrich Müller |
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Institution: | Paul Klingelhöfer,Ulrich Müller |
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Abstract: | Adducts of Oxotetrachloro-niobate (V). Formation, Vibrational Spectra, and Crystal Structures of PPh4NbOCl4(OH2)] and (PPh4)2NbOCl4(O2PCl2)] · 2 CH2Cl2 Crystalline (PPh4)2NbOCl4(O2PCl2)] · 2 CH2Cl2 was obtained by hydrolysis of PPh4NbSCl4] in the presence of POCl3 in CH2Cl2. Experiments to obtain the same compound from PPh4Cl, POCl3, NbCl5, and H2O yielded PPh4NbOCl4(OH2)]. I.R. spectra of both compounds are discussed. The crystal structure determinations with X-ray diffraction data in both cases show quadratic-pyramidal NbOCl4? ions to which a molecule of either H2O or a PO2Cl2? ion is attached in trans-position to the O atom. PPh4NbOCl4(OH2)]: tetragonal, space group P4/n, a = 1 308, c = 734 pm, Z = 2, packing as in the AsPh4RuNCl4] type; refinement down to R = 0.046 for 681 reflexions. (PPh4)2NbOCl4(O2PCl2)] · 2 CH2Cl2: triclinic, space group P1 , a = 1172, b = 1187, c = 2105 pm, α = 88.40, β = 83.20, γ = 71.28°, Z = 2, packing similar as in (AsPh4)2NbOCl5] · 2 CH2Cl2; refinement to R = 0.059 for 2 502 reflexions. |
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