The Combination of Organometallic {Mo(η³-allyl)(CO)₂(phen)} Fragments and Hard Aquo and Hydroxo Ligands:  Controlled Synthesis and Structural Characterization

The reaction of [Mo(η 3 -C 3 H 4 -Me-2)Cl(CO) 2 (phen)] with NaBAr‘ 4 (Ar‘ = 3,5-bis(trifluoromethyl)phenyl) and H 2 O allowed the isolation of the aquo complex [Mo(η 3 -C 3 H 4 -Me-2)(OH 2 )(CO) 2 (phen)]BAr‘ 4 ·2Et 2 O ( 1 ). Deprotonation of 1 afforded a neutral monomeric hydroxo compound isolated as [{Mo(η 3 -C 3 H 4 -Me-2)(OH)(CO) 2 (phen)} 2 (μ-H 2 O)] ( 2 ), which could be also obtained by reaction of [Mo(η 3 -C 3 H 4 -Me-2)Cl(CO) 2 (phen)] with KOH in a biphasic CH 2 Cl 2 /H 2 O medium. The reaction of 1 and 2 afforded the binuclear hydroxo-bridged compound [{Mo(η 3 -C 3 H 4 -Me-2)(CO) 2 (phen)} 2 (μ-OH)]BAr‘ 4 ( 3b ) via nucleophilic substitution of water by the hydroxo ligand.