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15 An excess of rhodium complex allows the coordination equilibration to be displaced and, thus, to complete the conversion of 1.
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31P NMR spectroscopy). Orange crystals of 2 (38 mg, 52%) were obtained by cooling the ether solution to -80 °C. Mp: 75 °C dec.
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33
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0013002082
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note
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2; 0.12 mmol) at room temperature. After the mixture was stirred for 30 min at this temperature, 1 mL of pentane was added and yellow crystals of 3 (60 mg, 64%) were obtained by cooling the solution to -20 °C. Mp: 63 °C dec.
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34
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0013017967
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note
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PRh = 224 Hz).
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35
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note
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27 All non-hydrogen atoms were treated anisotropically. The hydrogen atoms were geometrically idealized and refined using a riding model. Crystallographic data (excluding structure factors) have been deposited with the Cambridge Crystallographic Data Centre as Supplementary Publication Nos. CCDC-203087 (2), 203088 (3), and 203089 (3′). Copies of the data can be obtained free of charge on application to the CCDC, 12 Union Road, Cambridge CB2 1 EZ, U.K. (fax, (+44)1223-336-033; email, deposit@ccdc.cam.ac.uk).
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An investigation of the molecular structure of the mesityl analogue of 3 has been undertaken, and all relevant crystallographic data are reported in the Supporting Information. An geometry identical with that observed for 3 was determined. It should be noted that the mesityl derivative 3′ was considerably more reactive than 3, making its characterization much more difficult.
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