2009
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Abstract: Dinuclear [Cu(2)(R-pybox)(2)][X](2) [X = PF(6), R-pybox = 2,6-bis[4'-(S)-isopropyloxazolin-2'-yl]pyridine (S,S)-(i)Pr-pybox (1), 2,6-bis[4'-(R)-phenyloxazolin-2'-yl]pyridine) (R,R)-Ph-pybox (2), 2,6-bis[4'-(S)-isopropyl-5',5'-difeniloxazolin-2'-yl]pyridine (S,S)-(i)Pr-pybox-diPh (3); X = OTf, (R,R)-Ph-pybox (4)] and mononuclear complexes [Cu(R-pybox)(2)][PF(6)] [R-pybox = (S,S)-(i)Pr-pybox (5), (R,R)-Ph-pybox (6)] have been diastereoselectively prepared by reaction of [Cu(MeCN)(4)][PF(6)] or CuOTf.0.5C(6)H(6) … Show more

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“…The Cu-Cu distance [2.7430(11) Å] is consistent with nonbonding Cu-Cu contacts [14] and is similar to that found for the precursor 1 [2.7292(12) Å]. [5] Remarkably, the pybox skeleton is not planar with a torsion angle [N(2)-C(7)-C(6)-N(1)] of 31.2(10)°. The Cu-P distance is 2.2776 Å on average, which is comparable to those observed in other dinuclear copper(I) complexes containing μ-dppm ligands.…”
Section: Reaction Of [Cu 2 (R-pybox) 2 ][Pf 6 ] 2 (1 and 2) With Bidesupporting
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“…The Cu-Cu distance [2.7430(11) Å] is consistent with nonbonding Cu-Cu contacts [14] and is similar to that found for the precursor 1 [2.7292(12) Å]. [5] Remarkably, the pybox skeleton is not planar with a torsion angle [N(2)-C(7)-C(6)-N(1)] of 31.2(10)°. The Cu-P distance is 2.2776 Å on average, which is comparable to those observed in other dinuclear copper(I) complexes containing μ-dppm ligands.…”
Section: Reaction Of [Cu 2 (R-pybox) 2 ][Pf 6 ] 2 (1 and 2) With Bidesupporting
“…While the former anionic ligand produced [5] the dinuclear complex [Cu 2 (μ-Cl){(S,S)-iPr-pybox} 2 ][PF 6 ], the latter ligand gave a complex mixture from which only [Cu(CϵCPh)] n could be characterized. At this point, we turned our attention to the behavior of complexes 1 and 2 towards neutral ligands.…”
Section: Resultsmentioning
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“…To obtain more information on the reactive species of the real copper catalyst, we prepared the copper-pybox complex [Cu 2 (L1) 2 (m-Cl)][CuCl 2 ] [13,14] (4) from the reaction of CuCl with 0.7 equivalents of L1 in acetone at room temperature for 24 hours (Scheme 1 a). The molecular structure of 4 was unambiguously characterized by X-ray crystallography, and an ORTEP drawing of the cationic part of 4 is shown in A proposal of the dicopper complex, such as 4, as a reactive species in the present propargylation is also supported by a nonlinear relationship [15] between the ee value of optically active ligand L1 and the ee value of 3 a, which is produced by treatment of 1 a with 2 a in methanol at 0 8C for 48 hours in the presence of 5 mol % of CuOTf·1/2 C 6 H 6 and 10 mol % of L1 as shown in Scheme 1 c. This result provides direct evidence that a dinuclear copper complex works as a key reactive species in the propargylation.…”
Section: Entry 2)mentioning