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Convenient Synthesis of N‐Trimethylsilylaminotitanium Trichlorides
Author(s) -
Wrackmeyer Bernd,
Weidinger Jürgen,
Milius Wolfgang
Publication year - 1998
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/(sici)1521-3749(199801)624:1<98::aid-zaac98>3.0.co;2-d
Subject(s) - chemistry , trimethylsilyl , tin , crystal structure , stereochemistry , amide , dimer , medicinal chemistry , crystallography , organic chemistry
Bis(N‐trimethylsilylamino)plumbylenes 1 {[Me 3 Si(R)N] 2 Pb with R = t Bu ( a ), Me 3 Si ( b ), 9‐(9‐borabicyclo[3.3.1]nonyl) ( c )} react smoothly with an excess of TiCl 4 to give PbCl 2 and N‐trimethylsilylaminotitanium trichlorides 3 a – c . In contrast, the analoguous reaction of the corresponding stannylenes 2 a – c leads to mixtures containing unidentified Ti III compounds, the amides 3 a or 3 b , bis[bis(trimethylsilyl)amino]titanium dichloride 4 b and bis(amino)tin dichlorides 5 a – c . The crystal structure of 3 a was determined by X‐ray structural analysis. Compound 3 a is a dimer in the solid state with distorted trigonal pyramidal surroundings of the titanium atoms. Each titanium atom bears two μ 2 ‐Cl ligands which are in axial (d Ti–Cl = 250.7(1) pm) and equatorial positions (d Ti–Cl = 247.0(1) pm) and two terminal chloro ligands, one in axial (d Ti–Cl = 228.0(1) pm) and one in equatorial position (d Ti–Cl = 221.1(1) pm). The equatorial Ti–N bonds are short (183.8(2) pm).