in hexane
Mo2(O-i-Pr)6 was dissolved in hexane under N2. At room temp., chlorotrimethylsilane was added. The mixt. was then kept at 38°C (12 h).; The vol. of the soln. was reduced by half and cooled to -15°C. Crystals were obtained after 3 d. A second crop of crystals was obtained by reducing the vol. of the filtrate and cooled to -15°C.;
参考文献
Chisholm, Malcolm H.; Clark, David L.; Errington, R. John; Folting, Kirsten; Huffman, John C.
Inorganic Chemistry, 1988 , vol. 27, p. 2071 - 2084
in hexane
Mo2(O-i-Pr)6 was dissolved in hexane soln. under N2. At room temp., bromotrimethylsilane was added with stirring. After 2 h the soln. had changed color from yellow to burgundy, indicating the formation of Mo4Br3(O-i-Pr)9.; The vol. of the soln. was reduced by half and cooled to -15°C. Crystals were obtained after 3 d. A second crop of crystals was obtained by reducing the vol. of the filtrate and cooling to -15°C.;
参考文献
Chisholm, Malcolm H.; Clark, David L.; Errington, R. John; Folting, Kirsten; Huffman, John C.
Inorganic Chemistry, 1988 , vol. 27, p. 2071 - 2084
Prishchenko, A. A.; Gromov, A. V.; Luzikov, Yu. N.; Borisenko, A. A.; Lazhko, E. I.; et al.
J. Gen. Chem. USSR (Engl. Transl.), 1984 , vol. 54, # 7 p. 1520 - 1527,1354 - 1360
in hexane
Mo2(O-i-Pr)6 was dissolved in hexane. This soln. was cooled to -21°C, and then a hexane soln. of iodotrimethylsilane was added to the stirring soln.. The soln. was stirred at -21°C for 2 h.; The soln. was then allowed to warm to room temp. and stirred another 4 h, to yield a microcrystalline ppt.. The mixt. was then cooled to -15°C, and small crystals were isolated after 1 d.;
参考文献
Chisholm, Malcolm H.; Clark, David L.; Errington, R. John; Folting, Kirsten; Huffman, John C.
Inorganic Chemistry, 1988 , vol. 27, p. 2071 - 2084
