Ru3 CO 10 CN-f-Bu PMe2Ph

After the reaction is determined to be complete, solvent is removed (rotary evaporator), and the resulting deep red oil is extracted with two 10-mL aliquots of warm ( 40 °C) petroleum ether (boiling range, 40-60 °Q. The extracts are filtered, concentrated to 5 mL under vacuum, and cooled at — 10°C overnight to give Ru3(CO)10(CN-f-Bu)(PMe2Ph) (0.052 g, 42%) as deep red crystals. 

The complex is obtained as an orange microcrystalline solid [mp 150°C (dec)], which is readily soluble in acetone, dichloromethane, chloroform, and THF, but only sparingly soluble in light petroleum ether, cyclohexane, and methanol. The IR spectrum (cyclohexane) shows v(CO) bands at 2102 (m), 2068 (sh), 2052 (vs), 2034 (s), 2021 (vs), 2005 (sh), 1997 (w), 1987 (sh), and 1970(w)cm 1. A broad multiplet at 8 7.50 (Ph) is the only resonance in the HNMR spectrum (CDC13). 

UNDECACARBONYLTETRAHYDRIDO[TRIS(4-METHYL-PHENYL) PHOSPHITE]TETRARUTHENIUM, Ru4H4(CO)u[P(OC6H4Me-/ )3] 

The reaction mixture is transferred to a 50-mL round-bottomed flask and solvent is removed (rotary evaporator). The oily residue is dissolved in 2 mL of benzene and 8 mL of absolute ethanol is added. The mixture is kept in a freezer for 24 h. The bright yellow crystals that form are collected on a glass sinter and vacuum dried (1 torr, 25 °C). Yield 0.20 g (66%). 

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