Titan-stickstoff-verbindungen

Autor: K. Wiegel, D.J. Brauer, H. Bürger
Rok vydání: 1978
Předmět:
Zdroj: Journal of Organometallic Chemistry. 150:215-231
ISSN: 0022-328X
DOI: 10.1016/s0022-328x(00)84724-5
Popis: Novel cyclotrisilazane complexes X2Ti[N(SiMe2NMe)2SiMe2]2, X = Cl, Br and C6H5CH2 (VI), and chelate amido compounds (C6H5CH2)2Ti(NMeSiMe2)2 Y, Y = −, NMe and CH2, have been prepared and were characterized by 1H NMR and, in part, infrared and Raman spectroscopy. Pyrolysis of the bis(benzyl) derivatives apparently proceeds by an ionic mechanism, VI being remarkably stable with decomposition above 140°C. The crystal structure of VI was determined by single crystal X-ray methods. The compound forms triclinic crystals with a 14.629(3), b 17.461(4), c 17.593(2) A, α 88.447(8), β 80.673(8), γ 70.92(2)°, Z 4, P 1, D o 1.14 and D c 1.147 g cm −3 . Large block least-squares refinement, only the Ti and Si atoms are anisotropic, converged with an R index of 0.108 for 4820 counter measured reflections with I ⩾ 2σ(I). The Ti atoms possess distorted tetrahedral coordination with bond distances TiN 1.92(2) A, and TiC 2.09(3) A, and bond angles NTiN 120(1)° and CTiC 99(1)°. The large TiCC valency angles (117(1)–129(1)°) are indicative of the σ nature of the TiC(benzyl) bond. The cyclotrisilazane ligands have a boat conformation.
Databáze: OpenAIRE