Al; AlCl3 in tetrahydrofuran; ethylene glycol dimethyl ether (under Ar, Schlenk); flask charged with Al, AlCl3, ligand added, stirredat room temp. for 1 h, MoCl5 added, heated at 135°C for 30 h, co oled, mixt. of THF-DME added, refluxed for 6 h, cooled to room temp.; ppt. filtered, solvent removed in vacuo, ppt. dissolved in heptane, filtered, heptane stripped off, solid sublimed at 130°C/0.01 mmHg;

co-condensation of Mo-atoms and vapor of org. compd. (-196°C); according to: F. W. S. Benfield, M. L. H. Green, J. S. Ogden, D. Young, J. Chem. Soc., Chem. Commun., (1973) 866; vac. sublimation;