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(a) Matano, Y.; Begum, S. A.; Miyamatsu, T.; Suzuki, H. Organometallics 1998, 17, 4332-4334.
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Begum, S.A.2
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36
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0001108890
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Matano, Y, Begum, S. A, Miyamatsu, T, Suzuki, H. Organometallics 1999, 18, 5668-5681, Typical procedure: To a CH2Cl2 solution (10 mL) containing 1a (0.52 g, 1.0 mmol) and 1-pyrenylboronic acid (0.27 g, 1.1 mmol) was added BF 3·OEt2 (0.23 mL, 2.0 mmol) at 0°C, and the mixture was stirred for 2 h at room temperature. An aqueous solution of NaSbF6 (5.2 g, 20 mmol) was then added, and the resulting two-phase solution was vigorously stirred for 20 min. The aqueous phase was separated and extracted with CH2Cl2. The combined organic extracts were dried over MgSO4, passed through a short silica gel column, and evaporated under reduced pressure to leave a solid residue, which was recrystallized from CH2Cl2-Et2O to afford 2a·SbF6 0.87 g, 95, as a pale yellow solid. Bismuthonium salts 2·X are the
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6 (0.87 g, 95%) as a pale yellow solid. Bismuthonium salts 2·X are thermally stable (Mp ≥ 176°C) and can be kept as a solid state for more than 1 year in the dark.
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37
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59849120119
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2a·BF4: C37H30BBiF 4, monoclinic, P21/c, a, 9.779(3) Å, b, 19.034(5) Å, c, 16.871(5) Å, β, 102.501(1)°, V, 3065.8(15) Å3, Z, 4, Dc, 1.669 g cm-3, 6979 independent, 389 variables, R, 0.0545 (I > 2.00σ(I, wR, 0.1021, GOF, 1.041. 2a·SbF6: C37H 30BiF6Sb, triclinic, P1, a, 9.309(3) Å, b, 12.507(4) Å, c, 14.931(5) Å, α, 80.043(12)°, β, 80.653(13)°, γ, 73.665(12)°, V, 1631.1(10) Å3, Z, 2, Dc, 1.872 g cm-3, 7093 independent, 407 variables, R, 0.0408 (I > 2.00σI, wR, 0.0743, GOF, 1.039
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-3, 7093 independent, 407 variables, R = 0.0408 (I > 2.00σ(I)), wR = 0.0743, GOF = 1.039.
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38
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59849085506
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The distances between the bismuth and the nearest fluorine atoms are 4.4-4.5 Å.
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The distances between the bismuth and the nearest fluorine atoms are 4.4-4.5 Å.
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39
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59849087656
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6 [342 (270), 352 (310), 358 (300), 377 (96)].
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6 [342 (270), 352 (310), 358 (300), 377 (96)].
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40
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0000139666
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2 were determined as 0.04, 0.02, and 0.02, respectively, by comparison with that of pyrene (0.38) in the same solvent: Karpovich, D. S.; Blanchard, G. J. J. Phys. Chem. 1995, 99, 3951-3958.
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2 were determined as 0.04, 0.02, and 0.02, respectively, by comparison with that of pyrene (0.38) in the same solvent: Karpovich, D. S.; Blanchard, G. J. J. Phys. Chem. 1995, 99, 3951-3958.
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41
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23544472395
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2. For example, see: (a) Carmalt, C. J.; Norman, N. C.; Orpen, A. G.; Stratford, S. E. J. Organomet. Chem. 1993, 460, C22-C24.
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2. For example, see: (a) Carmalt, C. J.; Norman, N. C.; Orpen, A. G.; Stratford, S. E. J. Organomet. Chem. 1993, 460, C22-C24.
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42
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0000153329
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(b) Matano, Y.; Miyamatsu, T.; Suzuki, H. Organometallics 1996, 15, 1951-1953.
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Matano, Y.1
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Suzuki, H.3
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43
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0000887799
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Hatchard, C. G.; Parker, C. A. Proc. R. Soc. London, Ser. A 1956, 235, 518-536.
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Hatchard, C.G.1
Parker, C.A.2
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