Syntheses and Characterization of Chemically Flexible, Water-Soluble Dithio−Bis(phosphine) Compounds: (HOH2C)2P(CH2)2S(CH2)3S(CH2)2P(CH2OH)2, (HOH2C)2PCH2CH2S(CH2)4SCH2CH2P(CH2OH)2, and (HOH2C)2PCH2CH2CH2S(CH2)3SCH2CH2CH2P(CH2OH)2. Systematic Investigation of the Effect of Chain Length on the Coordination Chemistry of Rhenium(V). X-ray Crystal Structures of [ReO2(HOH2C)2P(CH2)2S(CH2)3S(CH2)2P(CH2OH)2]2(Cl)2, [ReO2(HOH2C)2P(CH2)2S(CH2)4S(CH2)2P-(CH2OH)2]2(ReO4-)2, and [ReO2(HOH2C)2P(CH2)3S(CH2)3S(CH2)3P(CH2OH)2](Cl)
Charles J. SmithKattesh V. KattiWynn A. VolkertLeonard J. Barbour
Abstract
The water-soluble dithio−bis(phosphine)s (HOH2C)2P(CH2)2S(CH2)3S(CH2)2P(CH2OH)2 (1), (HOH2C)2PCH2CH2S(CH2)4SCH2CH2P(CH2OH)2 (4), and (HOH2C)2PCH2CH2CH2S(CH2)3SCH2CH2CH2P(CH2OH)2 (7) were synthesized in near-quantitative yield by the formylation of their appropriate phosphine hydride precursors in the presence of formaldehyde and oxygen-free ethanol. The reactions of 1, 4, and 7 with [ReO2(C5H5N)4](Cl) in refluxing water produced the water-soluble Re(V) complexes [ReO2(HOH2C)2P(CH2)2S(CH2)3S(CH2)2P(CH2OH)2]2(Cl)2 (8), [ReO2(HOH2C)2P(CH2)2S(CH2)4S(CH2)2P(CH2OH)2]2(ReO4-)2 (9), and [ReO2(HOH2C)2P(CH2)3S(CH2)3S(CH2)3P(CH2OH)2](Cl) (10). The X-ray crystallographic analysis of 8−10, reported in this paper, confirmed the dioxorhenium(V) structures. All of the compounds were characterized by 1H, 13C, and 31P NMR spectroscopy. HPLC chromatographic analysis of 8−10 demonstrated purities of >98% for each of the new complexes formed. X-ray data for [ReO2(HOH2C)2P(CH2)2S(CH2)3S(CH2)2P(CH2OH)2]2(Cl)2 (8): monoclinic, P21/n, a = 10.7982(5) Å, b = 23.486(1) Å, c = 15.4408(8) Å, β = 94.539(1)°, Z = 4, R = 0.0246 (wR2 = 0.0574). For [ReO2(HOH2C)2P(CH2)2S(CH2)4S(CH2)2P(CH2OH)2]2(ReO4-)2 (9): triclinic, P1̄, a = 10.3762(5) Å, b = 12.1099(6) Å, c = 18.7555(9) Å, α = 90.259(1)°, β = 91.900(1)°, γ = 104.965(1)°, Z = 2, R = 0.0546 (wR2 = 0.1412). For [ReO2(HOH2C)2P(CH2)3S(CH2)3S(CH2)3P(CH2OH)2](Cl) (10): monoclinic, P21/n, a = 10.6224(6) Å, b = 12.5532(8) Å, c = 18.5767(11) Å, β = 103.663(10)°, Z = 4, R = 0.0261 (wR2 = 0.0656).
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