The reaction of the water-soluble monophosphine tris(hydroxymethyl)phosphine (THP, 1 ) with [ReO 2 (py) 4 ]Cl produced either trans,trans,trans -[ReO 2 (THP) 2 (py) 2 ]Cl ( 3, referred to as trans -[ReO 2 (THP) 2 (py) 2 ]Cl throughout the text) or trans,cis,cis -[ReO 2 (THP) 2 (py) 2 ]Cl ( 4, referred to as cis -[ReO 2 (THP) 2 (py) 2 ]Cl throughout the text) depending on the reaction conditions. In contrast, the reaction of THP with ReO 2 I(PPh 3 ) 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 [ReO 2 (py) 4 ]Cl produced the trans,trans,trans -[ReO 2 {PPh(CH 2 OH) 2 } 2 (py) 2 ]Cl complex ( 6, referred to as trans -[ReO 2 {PPh(CH 2 OH) 2 } 2 (py) 2 ]Cl throughout the text) in high yields. All compounds were characterized by 31 P, 1 H, and 13 C NMR spectroscopy and mass spectroscopy. X-ray data for 3: monoclinic, C 2/ 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 ( R w = 0.0426). X-ray data for 4: monoclinic, P 2 1 / 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 ( R w = 0.0483). X-ray data for 5: monoclinic, P 2/ 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 ( R w = 0.0887). X-ray data for 6: monoclinic, P 2 1 / 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 ( R w = 0.0578).
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Berning et al. (1998) studied this question.
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