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[Ti 3 Cl 8 (NPMe 3 ) 3 ]Cl has been prepared by the reaction of TiCl 3 (THF) 3  with Me 3 SiNPMe 3  in dichloromethane forming green moisture sensitive crystals. According to the crystal structure determination the titanium atoms of the cation [Ti 3 Cl 8 (NPMe 3 ) 3 ] +  are linked by two μ 3 -N atoms of two NPMe 3  -  groups forming a distorted trigonal-bipyramidal arrangement. The third NPMe 3  -  group and two of the chlorine atoms have μ2-bridging functions. The mixed-valence complex [V 2 Cl 4 (NPPh 3 ) 3 ] is formed as dark green moisture sensitive crystals by the reaction of vanadium trichloride with Me 3 SiNPPh 3  in boiling toluene. According to the crystal structure determination the vanadium atoms are linked by two μ 2 -N atoms of two NPPh 3  -  groups forming a nonplanar V 2 N 2  four-membered ring with a V-V distance of 266.8(1) pm which corresponds to a (σ, 1/2π) bond type. This is confirmed by the measurement of the magnetic susceptibility which leads to a magnetic moment of 1.45(5) B. M., corresponding to the remaining d 1  -electron.

zeitschrift für naturforschung b

Die Kristallstruckturen der Phosphaniminato-Komplexe.[Ti 3  IV Cl 8 (NPMe 3 ) 3 ]Cl und [V 2  III/IV Cl 4 (NPPh 3 ) 3 ]/Crystal Structures of the Phosphoraneiminato Complexes [Ti 3  IV Cl 8 (NPMe 3 ) 3 ]Cl and [V 2  III/IV Cl 4 (NPPh 3 ) 3 ]