in dichloromethane
under N2 atm. Ni3(depa)4Cl2 and AgPF6 in CH2Cl2 were stirred at -78°C in the dark for 1 h; soln. was filtered, layered with hexane and kept in freezer for 1 week; elem. anal.;
参考文献
Berry, John F.; Cotton, F. Albert; Lu, Tongbu; Murillo, Carlos A.; Wang, Xiaoping
Inorganic Chemistry, 2003 , vol. 42, # 11 p. 3595 - 3601
in neat (no solvent)
placing Se in a Pyrex ampoule; evacuation; condensing dry CH2Cl2 onto the Se; sealing the ampoule; heating to 570°C for 1h; Se is sublimed away, HCl and CH2Cl2 are pumped of at -80°C, residue is purified in vacuo by fractional condensation in traps held at -20, -90 and -198°C; CSe2 was cooled in the -90.gedree.C trap; stored at -198°C;
参考文献
Buerger, Hans; Willner, Helge
Journal of Molecular Spectroscopy, 1988 , vol. 128, p. 221 - 235
