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1
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For reviews of unique three-membered ring systems of heavier group 14 elements, see: a
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For reviews of unique three-membered ring systems of heavier group 14 elements, see: a) A. Sekiguchi, V. Ya. Lee, Chem. Rev. 2003, 103, 1429.
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N. Tokitoh, W. Ando, N. Choi, in Comprehensive Heterocyclic Chemistry II, ed. by A. R. Katritzky, C. W. Rees, E. F. V. Scriven, ed. by A. Padwa, Pergamon, Oxford, 1996, 1A, pp. 259-276.
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a) N. Tokitoh, W. Ando, N. Choi, in Comprehensive Heterocyclic Chemistry II, ed. by A. R. Katritzky, C. W. Rees, E. F. V. Scriven, vol. ed. by A. Padwa, Pergamon, Oxford, 1996, Vol. 1A, pp. 259-276.
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34250178516
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N. Tokitoh, N. Choi, W. Ando in Comprehensive Heterocyclic Chemistry II, ed. by A. R. Katritzky, C. W. Rees, E. F. V. Scriven, ed. by A. Padwa, Pergamon, Oxford, 1996, 1A, pp. 457-468, and references cited therein.
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b) N. Tokitoh, N. Choi, W. Ando in Comprehensive Heterocyclic Chemistry II, ed. by A. R. Katritzky, C. W. Rees, E. F. V. Scriven, vol. ed. by A. Padwa, Pergamon, Oxford, 1996, Vol. 1A, pp. 457-468, and references cited therein.
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6
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0035497126
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For the applications of dilithiosilane, see: a
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For the applications of dilithiosilane, see: a) M. Ichinohe, Y. Arai, A. Sekiguchi, N. Takagi, S. Nagase, Organometallics 2001, 20, 4141.
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Nakata, N.1
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12
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34250193362
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2: mp 156-157°C, 1H NMR (THF-d8, 298 K, δ) 0.26 (s, 6H, 1.10 (s, 18H, 1.13 (s, 18H, 1.56 (s, 6H, 1.61 (s, 6H, 1.68-1.78 (m, 6H, 13C NMR (THF-d8, 298 K, δ, 4.3, 16.8, 23.1, 23.3, 30.3, 30.6, 31.7, 35.3, 38.3, 39.1, 57.2, 58.6; 29Si NMR (THF-d8, 253 K, δ, 124.6, 8.5; 11B NMR (THF-d8, 298 K, δ) 50.1. 3: mp 179-180°C (dec, 1H NMR (THF-d8, 298 K, δ) 0.26 (s, 6H, 1.12 (s, 18H, 1.16 (s, 18H, 1.61 (s, 6H, 1.63 (s, 6H, 1.67-1.79 (m, 6H, 13C NMR (THF-d8, 298K, δ, 5.0, 15.6, 22.4, 22.8, 29.6, 29.9, 31.1, 34.5, 36.8, 37.5, 57.1, 58.0; 29Si NMR (THF-d8, 253 K, δ, 122.5, 10.5; 11B NMR (THF-d8, 298 K, δ) 52.5; 77Se NMR THF-d8, 298 K, δ, 400.7. Compun
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8, 298 K, δ) -400.7. Compunds 2 and 3 are unstable toward air and moisture. In particular, selenium derivative 3 decomposed to give a complicated mixture with liberation of red selenium.
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13
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0000986110
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a) R. P. Tan, G. R. Gillette, D. R. Powell, R. West, Organometallics 1991, 10, 546.
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34250193735
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Crystal data for 2: C27H60BNSSi3, MW 525.90, monoclinic, space group P21/m (no. 11, a, 8.4940(3, b, 17.5210(11, c, 11.4580(7) Å, β, 104.666(3)°, V, 1649.66(16) Å3, Z, 2, Dcalcd, 1.059 g cm-3, R 1 (I > 2σ(I, 0.0479, wR2 (all data, 0.1290 for 3006 reflections, 287 parameters, and 1 restraint, GOF, 1.031. 3: C27H60BNSeSi3, MW 572.80, monoclinic, space group P21/m (no. 11, a, 8.5350(3, b, 17.5160(10, c, 11.5160(6) Å3, β, 105.3430(3)̊, V, 1660.27(14) Å3, Z, 2, Dcalcd, 1.146 g cm-3, R1 (I > 2σ(I, 0.0377, wR2 all data, 0
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2 (all data) = 0.1012 for 3238 reflections and 284 parameters, GOF = 1.056. Selected bond lengths (Å) and angles (deg) for 3: Si1-B1 = 2.009(3), Si1-Se1 = 2.3355(7), Se1-B1 = 1.963(3), N1-B1 = 1.394(4), Se1-Si1-B1 = 53.09(9), Se1-B1-Si1 = 72.01(11), Si1-Se1-B1 = 54.90(9).
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0006892141
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34250204617
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4: mp 152-153°C, 1H NMR (C6D 6, 298 K, δ) 0.23 (s, 6H, 1.19 (s, 36H, 1.43 (s, 6H, 1.62 (s, 12H, 13C NMR (C6D6, 298 K, δ, 7.2, 17.2, 21.6, 29.5, 32.7, 42.1, 53.1; 29Si NMR (C6D 6, 298 K, δ, 2.5, 71.5; 11B NMR (C 6D6, 298 K, δ) 24.4. Compound 4 is moisture sensitive, giving insoluble white precipitates
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6, 298 K, δ) 24.4. Compound 4 is moisture sensitive, giving insoluble white precipitates.
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26
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34250200509
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2 (all data) = 0.1680 for 7813 reflections and 325 parameters, GOF = 0.995.
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2 (all data) = 0.1680 for 7813 reflections and 325 parameters, GOF = 0.995.
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28
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Supporting Information is available electronically on the CSJ-Journal Web Site, http://www.csj.jp/journals/chem-lett/.
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Supporting Information is available electronically on the CSJ-Journal Web Site, http://www.csj.jp/journals/chem-lett/.
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