Multifaceted Reactions of P(CH2OH)3 with Rhenium(V) Precursors. Synthesis, Characterization, and X-ray Structural Studies of trans,trans,trans-[ReO2{P(CH2OH)3}2- (py)2]Cl, trans,cis,cis-[ReO2{P(CH2OH)3}2(py)2]Cl, and Novel Alkoxide [Re(O)(μ-O)- (P{CH2OH}3)(μ-η2-P{CH2OH}2CH2O)]4
Citations Over TimeTop 10% of 1998 papers
Abstract
The reaction of the water-soluble monophosphine tris(hydroxymethyl)phosphine (THP, 1) with [ReO2(py)4]Cl produced either trans,trans,trans-[ReO2(THP)2(py)2]Cl (3, referred to as trans-[ReO2(THP)2(py)2]Cl throughout the text) or trans,cis,cis-[ReO2(THP)2(py)2]Cl (4, referred to as cis-[ReO2(THP)2(py)2]Cl throughout the text) depending on the reaction conditions. In contrast, the reaction of THP with ReO2I(PPh3)2 in biphasic media produced the novel, neutral, cyclic tetranuclear, rhenium(V) alkoxide 5 in low yields. A similar reaction of bis(hydroxymethyl)phenylphosphine (2) with [ReO2(py)4]Cl produced the trans,trans,trans-[ReO2{PPh(CH2OH)2}2(py)2]Cl complex (6, referred to as trans-[ReO2{PPh(CH2OH)2}2(py)2]Cl throughout the text) in high yields. All compounds were characterized by 31P, 1H, and 13C NMR spectroscopy and mass spectroscopy. X-ray data for 3: monoclinic, C2/c, a = 17.7964(11) Å, b = 8.8972(6) Å, c = 15.3247(9) Å, β = 97.683(1)°, Z = 4, R = 0.0179 (Rw = 0.0426). X-ray data for 4: monoclinic, P21/n, a = 12.1025(7) Å, b = 12.2670(7) Å, c = 15.5230(9) Å, β = 97.683(1)°, Z = 4, R = 0.0191 (Rw = 0.0483). X-ray data for 5: monoclinic, P2/c, a = 12.3759(7) Å, b = 9.8274(5) Å, c = 22.4272(12) Å, β = 96.807(1)°, Z = 2, R = 0.0437 (Rw = 0.0887). X-ray data for 6: monoclinic, P21/n, a = 9.3654(5) Å, b = 13.2578(7) Å, c = 12.0257(7) Å, b = 107.0480(10)°, Z = 2, R = 0.0218 (Rw = 0.0578).
Related Papers
- → Oxochloride Complexes of Rhenium(1971)22 cited
- → Design and Synthesis of Tunable Ligands with 4,4′-Bipyridyl as an Electron-Accepting Unit and Their Rhenium Complexes(2017)12 cited
- → Half-sandwich rhenium(III) acyl complexes: synthesis, structure and conversion to rhenium(I) and rhenium(III) isonitrile complexes(1996)14 cited
- → Rhenium-Oxo and Rhenium-Peroxo Complexes in Catalytic Oxidations(2007)33 cited
- → Syntheses and structures of trans-[ReX(CO)(Ph2PCH2PPh2)2] (X Cl, OReO3), including a rhenium(I)-rhenium(VII) complex(1993)10 cited