A large-scale synthesis of the benzophospholyl (BP) ligand, 4, has been developed and
employed in the synthesis of a series of manganese and iron complexes. Reaction between
Li-BP and FeCp(CO)2X (X = Br, I) resulted in the formation of [(μ2-BP)Fe2Cp2(CO)4]X, while
reaction of bis(1,1‘-benzophospholyl) with [FeCp(CO)2]2 gave a mixture of isomers of (μ2-BP)2Fe2Cp2(CO)2. The phosphine adduct (BP-Ph)Mn2(CO)9 was obtained from BP-Ph and
Mn2(CO)10 and converted to (η5-BP)Mn(CO)3 upon reaction with organometallic or organic
radicals. A synthesis for phenyl-iso-benzophosphole (iBP-Ph) has been explored. The
compound is highly reactive and polymerizes instantaneously and irreversibly. Polymerization of the iBP precursor was avoided in the novel partially hydrogenated derivative iBP-H2-Ph. Manganese complexes of iBP, 5, were obtained by reaction of iBP-H2-Ph with
Mn2(CO)10, resulting in the formation of (η5-iBP-H2)Mn(CO)3. Reaction of (η5-iBP-H2)Mn(CO)3 with DDQ gave (η5-iBP)Mn(CO)3, the first metal complex of iBP.
The title compound, [Mn2(C8H6P)(C14H11P)(CO)8], displays a novel coordination mode for a phospholyl ligand, where dinuclear coordination is observed through the P atom and the adjacent C atom of the heterocycle.
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