Kristallstrukturen von [TiF3(NPPh3)(HNPPh3)]2 und von HNPPh3 |
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Authors: | Marion Grün Klaus Harms Rolf Meyer Zu Kcker Kurt Dehnicke Helmut Goesmann |
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Institution: | Marion Grün,Klaus Harms,Rolf Meyer Zu Köcker,Kurt Dehnicke,Helmut Goesmann |
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Abstract: | Crystal Structures of TiF3(NPPh3)(HNPPh3)]2 and of HNPPh3 The phosphoraneiminato-phosphaneimine complex TiF3(NPPh3)(HNPPh3)]2 was obtained by the reaction of TiF4 with Me3SiNPPh3 in boiling dichloromethane. It crystallizes from 1,2-dichloroethane as yellow crystals which include four molecules C2H4Cl2 per dimeric formula unit. Space group P21/n, Z = 2, structure solution with 7270 independent reflections, R = 0.060 for reflections with I > 2σ(I). Lattice dimensions at ?50°C: a = 1417.5, b = 1896.9, c = 1586.6 pm, β = 101.22°. The compound forms centrosymmetric dimeric molecules via μ2-F bridges with TiF distances of 194.6 and 223.3 pm, the longer one being in trans-position to the N atom of the (NPPh3)? ligand. Its TiN bond length of 177.7 pm corresponds with a double bond. The TiN bond length of the HNPPh3 donor molecule of 213.4 pm is typical for a donor acceptor bond. According to the crystal structure determination the phosphaneimine HNPPh3 forms monomeric molecules without intermolecular hydrogen bridges with a PN bond length of 152.4 pm. Space group P21/c, Z = 4, structure solution with 3229 independent reflections, R = 0.062 for reflections with I > 2σ(I). Lattice dimensions at ?70°C: a = 1460.4, b = 928.9, c = 1096.6 pm, β = 93.35°. |
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Keywords: | Phosphorane Iminato-Phosphaneimine Complex of Titanium Synthesis Crystal Structure |
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