Water-soluble monophosphine P(CH 2 OH) 3 ( 1 ) and bisphosphines (HOH 2 C) 2 PC 6 H 4 P(CH 2 OH) 2 ( 2 ) and (HOH 2 C) 2 PCH 2 CH 2 P(CH 2 OH) 2 ( 3 ) were synthesized in near quantitative yields by the catalytic formylation of appropriate P−H bonded compounds in the presence of formaldehyde in aqueous media. The reactions of these mono- and bisphosphines 1−3 with ReO 2 I(PPh 3 ) 2, in biphasic media (aqueous/organic), or [ReO 2 (NC 6 H 5 ) 4 ]Cl, in aqueous media, produced the water-soluble Re(V) complexes [ReO 2 {P(CH 2 OH) 3 } 4 ] + ( 4 ), [ReO 2 {(HOH 2 C) 2 PC 6 H 4 P(CH 2 OH) 2 } 2 ] + ( 5 ), and [ReO 2 {(HOH 2 C) 2 PCH 2 CH 2 P(CH 2 OH) 2 } 2 ] + ( 6 ) in near quantitative yields. The X-ray structures of 5 and 6, reported in this paper, confirmed the dioxorhenium(V) structures of these new generation of water-soluble transition metal complexes. All the compounds were characterized by IR, 1 H, and 31 P NMR spectroscopy. X-ray data for 5: monoclinic, C 2/ c, a = 23.906(5) Å, b = 7.049(1) Å, c = 17.024(4) Å, β = 105.93(1)°, Z = 4, R = 0.019 ( R w = 0.027). For 6: triclinic, P 1̄, a = 6.493(1) Å, b = 9.488(2) Å, c = 10.577(2) Å, α = 104.4(1)°, β = 96.4(1)°, γ = 109.5(1)°, Z = 1, R = 0.045 ( R w = 0.060).
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Reddy et al. (1996) studied this question.
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