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Barron, A.R.1
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Nakamoto, M.1
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34548343385
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Spectral data for 2a: yellow crystals, mp 84-86°C (dec, 1H NMR (C6D6) δ-0.04 (s, 6H, 0.80 (s, 18H, 0.98 (s, 18H, 1.03 (s, 18H, 13CNMR (C6D 6) δ-7.61, 2.89, 22.1, 22.3, 25.1, 29.4 (2C, 34.0, 123.8-126.0 (m, 136.7 (d, 1J13C-19F, 248Hz, 138.5 (d, 1J13C-19F, 248Hz, 148.8 (d, 1J 13C-19F, 250 Hz, 29Si NMR (C6D6) δ 12.3, 18.5, 37.0. Spectral data for 2b: yellow crystals, mp 90-93°C (dec, 1HNMR (C6D6) δ, 0.01 (s, 6H, 0.79 (s, 18H, 0.90 (s, 18H, 1.02 (s, 18H, 13CNMR (C 6D6) δ, 7.48, 2.80, 21.7, 23.0, 26.6, 29.1 (2C, 33.9, 123.2-126.4 (m, 137.3 (d, 1J13C-19F, 245Hz, 138.5 (d, 1J13C-19F, 251 Hz, 149.4 d, 1J 13C-19F, 249Hz
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6) δ 17.1, 33.8, 47.8. The structure of 2b was unambiguously determined by X-ray crystallography; however, we do not discuss its structural features here because the refinement is not sufficiently good at this moment.
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20
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34548340106
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w = 0.1824 for all data) for 9761 reflections with I > 2σ(I). GOF = 1.056.
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w = 0.1824 for all data) for 9761 reflections with I > 2σ(I). GOF = 1.056.
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21
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0004204702
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3rd ed, Oxford University Press
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J. Emsley, The Elements, 3rd ed., Oxford University Press, 1998.
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(1998)
The Elements
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Emsley, J.1
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34548350679
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Spectral data for 4a: colorless crystals, mp 103-106°C, 1HNMR (C6D6) 8 0.10 (s, 3H, 0.18 (s, 3H, 0.98 (s, 18H, 1.09 (s, 18H, 1.21 (s, 18H, 1.32 (s, 6H, CH3CN, 13CNMR (C6D6) δ, 5.60, 1.54, 0.10 (CH3CN, 21.7, 22.3, 24.1, 29.9, 31.5, 34.1, 123.4-125.6 (m, 136.7 (d, 1J13C-19F, 245Hz, 137.6 (CH3CN, 138.6 (d, 1J13C-19F, 245Hz, 148.7 (d, 1J 13C-19F, 242Hz, 29SiNMR (C6D6) δ 5.87, 6.24, 11.6. Spectral data for 4b: colorless crystals, mp 109-111°C, 1HNMR (C6D6) δ 0.12 (s, 3H, 0.16 (s, 3H, 0.93 (s, 18H, 1.00 (s, 18H, 1.16 (s, 18H, 1.21 (s, 6H, CH3CN, 13CNMR (C6D6) δ0, 5.94, 1.96, 0.07 (CH3CN, 22.1, 22.3, 25.0, 29.3, 31.1, 33.5, 123.5-125.6 m
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6) 8 14.3, 19.4, 24.5.
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