Pure and Applied Chemistry

Pure Appl. Chem., 2010, Vol. 82, No. 3, pp. 603-612

http://dx.doi.org/10.1351/PAC-CON-09-08-02

Published online 2010-02-24

Synthesis and structure of stable 1,2-diaryldisilyne

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• 16. When THF was used as a solvent, disilyne 1 was obtained with an unidentified side product that was difficult to separate. No such side product was observed with the THF/Et₂O mixed solvent system.
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• 18. NMR spectral data of 5: ¹H NMR (300 MHz, C₆D₆): δ 0.23 (s, 18H), 0.32 (s, 18H), 0.36 (s, 18H), 0.36 (s, 54H), 0.43 (s, 18H), 1.97 (s, 2H), 5.93 (s, 2H), 6.95 (d, ⁴J_HH = 1.8 Hz, 2H), 7.00 (d, ⁴J_HH = 1.8 Hz, 2H); ¹³C NMR (75 MHz, C₆D₆): δ 1.05 (q), 1.52 (q), 1.60 (q), 2.28 (q), 5.13 (q), 22.73 (s), 24.39 (d), 29.63 (d), 124.57 (d), 128.01 (d), 133.62 (s), 148.12 (s), 148.38 (s), 157.26 (s); ²⁹Si NMR (59 MHz, C₆D₆): δ –25.1, 0.76, 0.99, 1.05, 1.59, 3.59.
• 19. Crystal data for [1_2C₇H₈]: C₇₄H₁₅₀Si₁₆, M = 1489.38, T = 103 (2) K, tetragonal, P4₂2₁2 (no. 94), 0.10 ? 0.05 ? 0.02 mm³, a = b = 16.6701(4) Å, c = 33.7498(11) Å, V = 9378.8(4) ų, Z = 4, D_calc = 1.055 g_cm^–3, μ = 0.252 mm^–1, 2θ_max = 50.0, 70 378 measured reflections, 8253 independent reflections (R_int = 0.1966), 446 refined parameters, GOF = 1.026, R₁ = 0.0723 and wR₂ = 0.1497 [I > 2σ(I)], R₁ = 0. 1762 and wR₂ = 0.2028 (for all data), largest diff. peak and hole 0.401 and –0.574 e.Å^–3.
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• 21. Frequency calculations were not performed at this stage because of the huge cost for computations.
• 22. Numerous reports describe theoretical studies of a disilyne and related compounds. For recent examples, see.
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• 23. Theoretical calculations for BbtGe?GeBbt (6) were performed at the B3PW91/6-311+G(2df)[Ge]: 6-31G(d)[Si,C,H] level. Although the basis sets for Si atoms of the substituents differ between the calculations for BbtGe?GeBbt and those for BbtSi?SiBbt, these results and discussions are reliable as a qualitative investigation.
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