Tungsten tetrachlorobis

P2CI4WC25H24, Tungsten(IV), tetiachloro-bis(methyldiphenylphosphine)-, 28 328 P2CI4WC3JH30, Tungsten, tetrachlorobis(tri-phenylphosphine)-, 28 40 P2CoC,H23, Cobaltp), (V-cyclopenta-dienyl)bis(trimethylphosphine)-,... 

Tetrachlorobis(triphenylphosphine)tungsten(IV) (4.5 g, 53 mmole) and 1,2-bis-(diphenylphosphino)ethane (2.1 g, 5.3 mmole) are heated in toluene (50 mL, distilled from sodium) at 70° for 3 hours in a 100-mL flask carrying a reflux condenser. The resulting yellow-green solid is filtered using a Schlenk filter, washed with toluene (30 mL) and diethyl ether (30 mL), and dried (10 2 torr, 20°). Yield 2.4 g, 89% it is sufficiently pure for subsequent preparations. Anal. Calcd. for C26H24C14P2W C, 43.1 H, 3.3. Found C, 44.5 H, 3.6. 

CUOW, Tungsten chloride oxide, 23 195 Cl402TiCiHlt, Titanium(IV), tetrachlorobis-(tetrahydrofuran)-, 21 135 C1402ZiC,H16, Zirchonium(IV), tctrachlorobis-(tetrahydrofuran)-, 21 136 Cl4P2C2H4, Phosphine, 1,2-ethanediylbis-(dichloro-, 23 141... 

Cl4Nb02CgH,g, Niobium, tetrachlorobis-(tetrahydrofuran)-, 29 120 CI4OW, Tungsten tetrachloride oxide,... 

Petroleum ether (100 mL) is added with a syringe to tetrachlorobis(l, 1-di-methylethanamine)bis[( 1,1 -dimethylethyl)imidobis(phenylimido)ditungsten-(VI) (2g, 2 mmol) contained in a 2S0-mL two-neck round-bottomed flask fitted with a gas inlet tap and a rubber serum cap. A solution of trimethyl phosphine (1.2 mL, 10.9 mmol) in petroleum ether (40 mL) in a 100-mL two-necked round-bottomed flask fitted with gas inlet tap and rubber septum is transferred to the suspension of the tungsten complex in petroleum ether. The serum cap is replaced by a greased glass stopper, and the mixture is stirred for at least 24 h. The dark red complex is removed by filtering, washed twice with petroleum ether (30 mL), and dried under vacuum. Yield 2.1 g (91%). 

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