in dichloromethane byproducts: CO; Dissolving of freshly prepd. Mn(CO)5(CBr3) and (PPN)(Co(CO)4) in CH2Cl2 at -78°C under N2, warming (30 min, room temp.) until end of CO evolution.; Evapn., extn. of solid with hexane (4x) to remove Mn(CO)5Br, extn. (i-Pr2O) of remaining solid, filtering, layering with pentane, dark brown solid forms, filtering, washing (pentane), drying in vac., elem. anal.;

in dichloromethane molar ratio Mn:Co=1:1.7; -78°C; slow warming to room temp.; removal of Mn(CO)5Br by extn. with hexane; cluster was extd. into Et2O;repeated recrystn. by slow diffusion of pentane into Et2O soln.; elem. anal.;

in tetrahydrofuran N2-atmosphere; stirring (room temp., 24 h), warming (60°C, 5-6 h); filtration, evapn. (reduced pressure), extn. (hexane, then toluene), repeated recrystn. of residue (CH2Cl2/hexane); elem. anal.;

in acetonitrile mixed; followed by IR, removal of solvent, extn. (hexane or benzene), sepn. by column or thin-layer chromy.;

sodium nitrite in tetrahydrofuran room temperature; solid NaNO2 was added; 15 min; evaporated in vacuo; recrystallized from acetone; elem. anal.;

in tetrahydrofuran The iron complex and Co(CO)8 are slurried in THF under CO (20 min).; Evapn., resulting oil is dissolved in Et2O, (PPN)Co(CO)4 is removed by filtration, addn. of 2-propanol, evapn. yields black/purple PPN-compound which is washed with pentane and dried by vac, elem. anal.;

(CH3)3NO*2H2O in acetonitrile addn. of a soln. of Me3NO*2H2O in freshly distilled MeCN to a soln. of Co-complex in MeCN, stirring at room temp. for 1 h, addn. of Mo-compd. in MeCN, stirring for 10 min, colour changes from purple/brown to green; removal of solvent, extn. into CH2Cl2, layering with Et2O to remove Co-Compd., filtn., layering with hexane to remove Mo-compd., concn. of soln. yields Co/Mo-complex, elem. anal.;

in dichloromethane N2-atmosphere; addn. of (PPN)Cl to Co/Rh complex, then addn. of 2 equivs. PEt3; solvent removal (vac.), hexane addn., filtration, washing (hexane);

CO in methanol; acetone Irradiation (UV/VIS); Co(acac)2 in acetone/methanol (4/1) under atmospheric pressure of CO, irradn. for 18 h, addn. to (Ph3P)2NCl, stirring 12 h, removal of solvent; recrystn. from MeOH/H2O;

in tetrahydrofuran byproducts: NH3; under N2, addn. of ammonium-salt to soln. of Co-complex; evapn. to dryness, addn. of CH2Cl2, stirring for 2 h, filtn., addn. of Et2O, crystn. at -40°C;