Wolframnitridchlorid‐Benzonitril, [WNCl3 · NC–Ph]4, entsteht durch Einwirkung von N,N,N'‐tris(trimethylsilyl)benzamidin auf Wolframhexachlorid in CCl4‐Lösung in Form roter Kristallnadeln, die wir IR‐spektroskopisch und durch eine röntgenographische Strukturanalyse charakterisiert haben. Die Verbindung kristallisiert monoklin in der Raumgruppe C2/c mit vier Formeleinheiten pro Elementarzelle (1983 unabhängige, beobachtete Reflexe, R = 7,5%). Die Gitterabmessungen sind bei 19°C: a = 1464,8; b = 1902,6; c = 2033,8 pm; β = 102,27°, Im [WNCl3 · NCPh]4 sind die Wolframatome an den Ecken eines Quadrats angeordnet und über alternierend lange lineare Nitridobrücken vom Typ WNW mit WN‐Abständen von (im Mittel) 166 bzw. 211 pm verknüpft. In trans‐Position zu den kurzen WN‐Bindungen befinden sich die N‐Atome der Benzonitrilliganden mit W–N‐Abständen von 237 pm.

N,N,N'-Tris(trimethylsilyl)benzamidine, [C6H5-C(NSiMe3)N(SiMe3)2], reacts with antimony trichloride in CH2Cl2 solution to form monomeric dichloroantimony-N,N'-bis(trimethylsilyl)- benzamidine, [SbCl2(NSiMe3)2C-C6H5]. Both benzamidine derivatives have been character­ized by crystal structure determinations. [C6H5-C(NSiMe3)N(SiMe3)2]: space group P21/c, Z = 4, 2278 observed independent refle­xions, R = 0,038. Lattice dimensions (19 °C): a = 1521,0(1); b = 656.7(1); c = 2163,0(1) β = 94,21(1)°. The compound forms monomeric molecules with CN distances of 126,6 pm, and 141,0 pm, respectively, corresponding to C=N̄-SiMe3 and C-N(SiMe3)2 moieties. [SbCl2(NSiMe3)2C-C6H5]: space group P21/c, Z = 4, 2707 observed independent reflexions, R = 0,027. Lattice dimensions (19 °C): a = 1212,7(1); b = 962,1(1); c = 1728,9(1) pm; β = 98,02(1)°. The compound forms monomeric molecules in which the antimony atom is surrounded by two chlorine atoms, and by the N atoms of the benzamidine chelate, forming a distorted trigonal bipyramidal arrangement, which is a consequence of the steric effect of the lone pair on the Sb atom.

Abstract The trichlorides of aluminium, gallium, and indium, as well as boron tribromide and tin tetra-chloride react with N,N,N'-tris(trimethylsilyl)benzamidine to form the monomeric N.N'-bis-(trimethylsilyl)benzamidinato complexes Ph-C(NSiMe3)2MX2(M = B, Al. Ga, In; X = Cl, Br) and Ph -C(NSiMe3)2SnCl3 , respectively. All compounds have been characterized by their IR spectra, two of them by X-ray diffraction studies. Ph - C(NSiMei)2AlCl2 : Space group C2/c, Z = 4, 1152 independent observed reflexions, R = 0.052. Lattice dimensions (19 °C): a = 1558.6(1), b = 1116.6(1), c = 1307.0(1) pm, β = 115.17(1)°. The compound forms monomeric molecules, in which the aluminium atom is tetra-hedrally coordinated by two chlorine atoms and by the two nitrogen atoms of the benzamidinato chelate. Bond length A1N = 188.2 pm. Ph - C(NSiMe3)2SnCU: Space group P1̄, Z = 2, 3293 independent observed reflexions, R = 0.034. Lattice dimensions (19 °C): a = 980.1(1), b = 1025.9(1), c = 1230.5(2) pm. a = 68.40(1)°, β = 87.71(1)°, y - 68.92(1)°. The compound forms monomeric molecules, in which the tin atom is five-coordinated by three chlorine atoms and by the two nitrogen atoms of the benzamidinato chelate. Bond lengths SnN = 213.5 and 215.2 pm.

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The novel title compound (III) has the space group P1 with Z=2.