Darstellung und Struktur neuer Calix[4]aren-Titan(IV)-Imidokomplexe

Synthesis and Structure of New Calix[4]arene Titanium(IV) Imido Complexes The syntheses of the novel calix[4]arene titanium imido compounds [Cax(OMe)₂O₂Ti(NR)] ( 2 ) (R = tBu) and ( 3 ) (R = Mes = 2,4,6-trimethylphenyl) (Cax = C₄₄H₅₂) starting from [Cax(OMe)₂O₂TiCl₂] ( 1 ) and lithium amides LiNHR are described. Complexes 2 and 3 are mononuclear compounds in solution. An X-ray crystal structure analysis of the toluene adduct of 3 (Space group: P 1, lattice dimensions: a = 12.979(2) Å, b = 13.707(2) Å, c = 16.573(3) Å, α = 81.751(11)°, β = 80.555(13)°, γ = 73.541(12)°) reveals that this compound is mononuclear in the solid state. The central atom in 3 is distorted trigonal bipyramidal ligated by two ether oxygen atoms in axial positions, two phenoxide oxygen atoms in the equatorial plane, and an imido nitrogen atom in an equatorial position. The titanium nitrogen bond distance in 3 is 171.8(3) pm.