The ligands [ n BuSn(2-pyridyl) 3 ] and [RSn(methylthiomethyl) 3 ] (R ) n Bu, Me) have been prepared in a one-pot, two-step procedure from the corresponding alkyltin trichloride and 2-pyridyl or methylthiomethyl carbanions. The reaction of these ligands with [M(CO) 3 (NCR) 3 ] (M ) Mo, W) afforded the tricarbonyl compounds [{ n BuSn(2-pyridyl) 3 }M(CO) 3 ] and [{RSn-(methylthiomethyl) 3 }M(CO) 3 ]. In addition to IR and NMR characterization, the structure of three of these new complexes was determined by single-crystal X-ray diffraction.
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 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.
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