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We noticed that compounds 4 exist as a mixture of cis- and transisomers in solution, and the ratio of isomers depended on the solvents. For example, the ratio of the two isomers changed from about 1:1 in CDCl 3 to about 3:1 in DMSO-d6. The )H nmr spectrum data are attached here: 4f (CDCl3, δ 9.31 (d, J, 2.1, 0.44H, 8.95 (d, J, 2.1, 0.56H, 8.51 (dd, J, 8.4, 2.4, 0.44H, 8.23 (dd, J, 8.4, 2.4, 0.56H, 8.21 (s, 0.56H, 8.00 (d, J, 8.1, 1.12H, 7.82 (d, J, 8.1, 0.88H, 7.57-7.40 (m, 4H, 7.23-7.09 (m, 3H, 6.93 (d, J, 8.1, 1H, 6.78 (s, 0.44H, 2.40 (s, 1.32H, 2.38 (s, 1.68H) ppm; 4f (DMSO-d6, δ 9.15 (d, J, 2.1, 0.25H, 8.81 (d, J, 2.1, 0.75H, 8.53 (dd, J, 8.4, 2.4, 0.25H, 8.31 (dd, J, 8.4, 2.4, 0.75H, 8.39 (s, 0.75H, 8.05 (d, J, 8.1, 1.5H, 7.82 (d, J, 8.1, 0.5H, 7.81-7.74 (m, 1H, 7.65-7.58 (m, 2H, 7.50-7.43 (m, 1H, 7.30-7.18 (m, 3.5H, 6.91 (d, J, 8.1, 0.5H, 6.58 s, 0.25H
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6): δ 9.15 (d, J = 2.1, 0.25H), 8.81 (d, J = 2.1, 0.75H), 8.53 (dd, J = 8.4, 2.4, 0.25H), 8.31 (dd, J = 8.4, 2.4, 0.75H), 8.39 (s, 0.75H), 8.05 (d, J = 8.1, 1.5H), 7.82 (d, J = 8.1, 0.5H), 7.81-7.74 (m, 1H), 7.65-7.58 (m, 2H), 7.50-7.43 (m, 1H), 7.30-7.18 (m, 3.5H), 6.91 (d, J = 8.1, 0.5H), 6.58 (s, 0.25H), 2.37 (s, 0.75H), 2.38 (s, 2.25H) ppm.
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Crystallographic data (excluding structure factors) for the structures in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication nos. CCDC 639095 (4c) & 635094 (8, Copies of the data can be obtained, free of charge, on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK, fax: +44-(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk
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Crystallographic data (excluding structure factors) for the structures in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication nos. CCDC 639095 (4c) & 635094 (8). Copies of the data can be obtained, free of charge, on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK, (fax: +44-(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk).
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