New route to complexes having substituted quinoline-2-thiolate ligands through the metal-assisted coupling and cyclization of aryl isothiocyanates to alkyne ligands
- Univ. of South Carolina, Columbia, SC (United States)
Reactions of the lightly stabilized dimetalated olefin complex Re(CO){sub 4}[trans-{mu}-HC=C(CO{sub 2}Me)]Re-(CO){sub 4}(NCMe) (1) with p-tolylisothiocyanate has yielded the complex Re(CO){sub 4}[(E)-HC=C(CO{sub 2}Me)C=N (C{sub 6}H{sub 4}-p-Me)S]Re(CO){sub 4} (2; 58% yield) by insertion of the isothiocyanate into the substituted Re-C bond. When 2 is treated with I{sub 2} in the presence of UV radiation, the tolyl ring cyclizes with the unsubstituted end of the metalated olefin to yield a new substituted quinoline-1-thiolate ligand in the complex Re{sub 2}(CO){sub 7}[{mu}-2-S-3-CO{sub 2-}Me-6-Me-NC{sub 9}H{sub 4}] ({mu}-I) (3; 18% yield). Complexes 2 and 3 were characterized by IR, {sup 1}H NMR, and single-crystal X-ray diffraction analyses. Crystal data: for 2, space group P2{sub 1}/c, a = 10.317 (1) {angstrom}, b = 15.819(2) {angstrom}, c = 15.448-(3) {angstrom}, {beta} = 103.26(1){degrees}, Z =4,2415 reflections, R = 0.027; for 3{center_dot}CH{sub 2}Cl{sub 2}, P{bar 1}, a = 10.204(4) {angstrom}, b = 13.733(6) {angstrom}, c = 9.877 (2) {angstrom}, {alpha} = 91.18(3){degrees}, {beta} = 96.17(3){degrees}, {gamma} = 74.78(3){degrees}, Z = 2,2746 reflections, R = 0.038.
- Sponsoring Organization:
- USDOE
- OSTI ID:
- 433543
- Journal Information:
- Organometallics, Vol. 12, Issue 7; Other Information: PBD: Jul 1993
- Country of Publication:
- United States
- Language:
- English
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