Synthese von Nitrenkomplexen mit N-Trimethylsilylanilin I. Charakterisierung und Kristallstruktur von [Re(NPh)Cl3(Et2PhP)2] und [Re(NPh)Cl3(Ph3P)2] ·1/2 CHCl3 / Synthesis of Nitrene Complexes with N –T rimethylsilylaniline I. Characterisation and Crystal Structure of [Re(NPh)Cl3(Et2PhP)2] and [Re(N Ph)Cl3(Ph3P)2] · 1/2CHCl3
2014
Wittern, Ursula | Strähle, Joachim | Abram, Ulrich
trans-mer--Trichlorobis(diethylphenylphosphine)phenylnitrene rhenium(V), [Re(NPh)Cl₃- (Et₂PhP)₂], has been synthesized from [ReOCl₃ (Et₂ PhP)₂ ] and N-trimethylsilylaniline, while trans-mer-trichlorophenylnitrenebis (triphenylphosphine) rhenium(V), [Re(NPh)Cl₃ (Ph₃P)₂] has been obtained via a novel route, from (Bu₄N)[ReOCl₄ ] and N-trimethylsilylanilin. The products were studied by mass spectrometry, IR spectroscopy and X-ray diffraction.trans-mer-[Re(NPh)Cl₃(Et₂PhP)₂ ] crystallizes in the monoclinic space group P2₁/n with a = 1498.5(3), b = 1068.6(1), c = 1784.0(4) pm and β = 91.28(1)°, Z = 4. The rhenium atom exhibits a distorted octahedral coordination with the phosphine groups in trans positions, and the Cl ligands in a meridional arrangement. The Re ≡N -C moiety is linear with a bond angle o f 169,4(5)°and a Re= N bond length o f 171.8(6) pm.[Re(NPh)Cl₃(Ph₃P)₂ ]· 0.5 CHCI₃ crystallizes in the triclinic space group P 1̄ with a = 1232.1 (4), b= 1431.6(5), c = 2236.6(8) pm, a = 89.19(2)°, β = 80.50(2)°and γ = 88.26(2)°, Z = 4. The asymmetric unit contains two symmetry independent complex molecules of approximately the same structure, with Cl atoms meridionally arranged and the phosphine groups in trans positions. The coordination geometry is a distorted octahedron. The almost linear Re≡N -C moieties have Re≡N bond lengths of 170.2(7) and 170.8(7) pm, respectively, and Re≡N -C angles of 173.3(6)°and 175.0(7)°.
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