CO in hexane Addn. of Ru3-complex to soln. of Ru(CO)5, heating to reflux under continuous purge with CO for 10 min, yellow soln. turns brown.; Concg., column chromy. (Florisil), eluation of Ru3(CO)12 with hexane, hexane/CH2Cl2 eluates Ru5-complex (elem. anal.) and later Ru6-complex.;

CO in n-heptane Addn. of Ru3-complex to soln. of Ru(CO)5, heating to reflux under continuous purge with CO for 15 min, yellow soln. turns brown.; Concg., column chromy. (Florisil), eluation of Ru3(CO)12 with hexane, hexane/CH2Cl2 eluates Ru5-complex , Ru6-complex (elem. anal.) and Ru7-complex (elem. anal.).;

CO in n-heptane High Pressure; 100 atm CO, 125°C, 4 h; concn., cooling (-20°C), filtration of Ru4(CO)11S2, chromy. of filtrate (Florisil, hexane), then thin layer chromy. (hexane; then hexane/CH2Cl2=4:1);

in hexane Irradiation (UV/VIS); (N2); to hexane soln. of Ru complex was added W compd. and stirred soln. was irradiated for 20 min, solvent removed in vac.; residue chromd. (TLC, hexane/CH2Cl2 85:15); elution order: 1. Ru3(CO)12, 2. main product; elem. anal., 3. Ru phosphino complex, elem. anal.;

With  CO in  octane  High Pressure; 100 atm CO, 125°C, 4 h; cooling to 25°C, crystn. (-25°C);   

 in  n-heptane  byproducts: Ru3(CO)12; Ru3(CO)10S was placed into a tube, heptane was added, the tube was sealed under vac., placed into an oil bath, the soln. was stirred vigorously at 100°C for 10 min, the tube was removed and cooled to 25°C; tube was opened, soln. was decanted, ppt. was extd. with CH2Cl2 yielded Ru4(CO)11S2, soln. was evapd. to dryness, residue was dissolved in hexane, chromd. with hexane, Ru3(CO)12 sepd., eluted with hexane/CH2Cl2 gave Ru7(CO)20S2 and Ru6(CO)17S2;   

 in  n-heptane  byproducts: Ru3(CO)12; Ru3(CO)10S was placed into a tube, heptane was added, the tube was sealed under vac., placed into an oil bath, the soln. was stirred vigorously at 100°C for 10 min, the tube was removed and cooled to 25°C; tube was opened, soln. was decanted, ppt. was extd. with CH2Cl2 yielded Ru4(CO)11S2, soln. was evapd. to dryness, residue was dissolved in hexane, chromd. with hexane, Ru3(CO)12 sepd., eluted with hexane/CH2Cl2 gave Ru7(CO)20S2 and Ru6(CO)17S2;   

 in  n-heptane  byproducts: Ru3(CO)12; Ru3(CO)10S was placed into a tube, heptane was added, the tube was sealed under vac., placed into an oil bath, the soln. was stirred vigorously at 100°C for 10 min, the tube was removed and cooled to 25°C; tube was opened, soln. was decanted, ppt. was extd. with CH2Cl2 yielded Ru4(CO)11S2, soln. was evapd. to dryness, residue was dissolved in hexane, chromd. with hexane, Ru3(CO)12 sepd., eluted with hexane/CH2Cl2 gave Ru7(CO)20S2 and Ru6(CO)17S2;