Syntheses, characterization, and structures of tri- and tetraruthenium clusters containing sulfido, phenylimido, and (phenylimino)thio ligands
- Northwestern Univ., Evanston, IL (United States)
Reaction of Ru{sub 3}(CO){sub 12} with the SO{sub 2} analog N-sulfinylaniline (PhN=S=O) in refluxing toluene produces Ru{sub 3}-(CO){sub 9}({mu}{sub 3}-NPh)({mu}{sub 3}-S) (1), Ru{sub 3}(CO){sub 9}({mu}{sub 3}-NPh){sub 2} (2), Ru{sub 4}(CO){sub 10}({mu}-CO)({mu}{sub 4}-{eta}{sup 2}-SNPh)({mu}{sub 4}-S) (3), and Ru{sub 4}(CO){sub 10}({mu}-CO)({mu}{sub 4}-{eta}{sup 2}-SNPh)({mu}{sub 4}-NPh) (4) in low yields. Treatment of Ru{sub 3}(CO){sub 10}(NCMe){sub 2} with PhN=S-O at room temperature affords 1 as the major product in good yield, accompanied by CO{sub 2} formation. Compounds 1, 3, and 4 were characterized by mass, IR, and {sup 1}H NMR spectroscopy, and their structures were determined by single-crystal X-ray diffraction. Crystal data for 1: triclinic (P1), a = 9.585(2) {angstrom}, b = 10.151(2) {angstrom}, c = 10.555(4) {angstrom}, {alpha} = 92.32(3){degrees}, {beta} = 93.21(3){degrees}, {gamma} = 98.84(2){degrees}, Z = 2, R (R{sub w}) = 0.026 (0.030). Crystal data for 3: monoclinic (P2{sub 1}/n), a = 8.986(7) {angstrom}, b = 13.968(3) {angstrom}, c = 19.232(9) {angstrom}, {beta} = 103.06(5) {angstrom}, Z = 4, R (R{sub w}) = 0.025 (0.025). Crystal data for 4: monoclinic (P2{sub 1}/c), a = 10.319(4) {angstrom}, b = 23.354(6) {angstrom}, c = 23.329(7) {angstrom}, {beta} = 100.43(3){degrees}, Z = 8, R (R{sub w}) = 0.051 (0.040).
- DOE Contract Number:
- FG02-86ER13540
- OSTI ID:
- 513371
- Journal Information:
- Inorganic Chemistry, Journal Name: Inorganic Chemistry Journal Issue: 26 Vol. 35; ISSN 0020-1669; ISSN INOCAJ
- Country of Publication:
- United States
- Language:
- English
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