in dichloromethane-d2 I2 was sublimed into the complex at 77 K after CH2Cl2, stored at -80°C and every 30 min heavily shaken for about 1 min (10 times), 4 days(inert atm.); ppt. was filtered at -80°C, volatiles were quickly removed at 0°C; elem. anal.;
参考文献
Krossing, Ingo
Journal of the Chemical Society, Dalton Transactions, 2002 , # 4 p. 500 - 512
trimethylsilyl iodide in carbon disulfide under N2, reaction of P4 with I2, followed by treatment of the soln. with (CH3)3SiI; not isolated, identified by 31P-NMR spectroscopy;
in carbon disulfide addition of I2 in CS2 in portions while swinging to filtered soln. of P4 in pure CS2, allowing stand for 12 h in dark to complete reaction and concentrating orange red soln. whith warming on water bath;; crystals are sucked off with glass frit and evacuated over CaCl2 until pressure of 20 Torr is reached;;
参考文献
Zeitschrift fuer Naturforschung, , vol. 13b, p. 266 - 267
