trimethylstannyl chloride in diethyl ether; toluene inert atmosphere; addn. of Me3SnCl to Li-salt in Et2O at -40°C, warming to room temp., evapn., addn. of ZrCl4 suspn. in toluene, stirring(80°C, 4 h); evapn. (80-90°C, 1 torr), recrystn. or washing;

in toluene under inert atm.; Zr-complex was dissolved in toluene, soln. of trichloroacetyl chloride in toluene was added, 1 h; petroleum ether was added, ppt. filtered off, recrystd. from THF and pentane, 2 d;

in THF-d8 (tetrahydrofuran-d8) 8 d, room temp.; reaction was monitored by (1)H NMR;

in tetrahydrofuran byproducts: (P-t-Bu)4, PH2-t-Bu; recrystn. from THF for several days; elem. anal.;

in benzene-d6 C6D6, 2-5-fold excess of Al-compound, room temp.; not sepd., detected by NMR spectra;