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77953869112
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EDBP)2 Mg, Na)2(THF)5]·THF (1, Yield 1.10 g (83, Anal. Calcd for C84H136MgNa2O10: C, 73.31; H, 9.96. Found: C, 72.74; H, 9.48. 1H NMR (CDCl3, ppm, δ 7.38 (s, 2H, Ph, 7.03 (m, 6H, Ph, 4.97 (q, 2H, CH(CH3, J, 7.2 Hz, 3.42 (s, 20H, O-CH2, 1.73 (s, 20H, CH2, 1.59 (d, 6H, CH(CH3, J, 7.2 Hz, 1.34 (s, 36H, C(CH3)3, 1.24 (s, 36H, C(CH3)3, 13C NMR (CDCl3, ppm, 158.70, 137.15, 135.77, 134.42, 121.29, 120.57 (Ph, 67.92 (O-CH2, 35.17, 34.07, 32.00, 30.47 (t-Bu, 29.79 (CH(CH3, 25.27 (CH2, 22.97 (CHCH3
-
3)).
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30
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77953872900
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EDBP)2 Mg, K)2(THF)5]·THF (2, Yield 1.17 g (87, Anal. Calcd for C84H136MgK2O10: C, 71.63; H, 9.73. Found: C, 72.01; H, 9.90. 1H NMR (CDCl3, ppm, δ 7.06 (s, 2H, Ph, 6.96 (m, 6H, Ph, 4.97 (q, 2H, CH(CH3, J, 7.2 Hz, 3.54 (s, 20H, O-CH2, 1.79 (s, 20H, CH2, 1.60 (d, 6H, CH(CH3, J, 7.2 Hz, 1.29 (s, 36H, C(CH3)3, 1.21 (s, 36H, C(CH3)3, 13C NMR (CDCl3, ppm, 160.09, 137.16, 134.98, 134.61, 121.76, 120.00 (Ph, 67.80 (O-CH2, 35.17, 34.03, 31.97, 31.55 (t-Bu, 30.07 (CH(CH3, 29.80 (CH2, 25.44 (CHCH3
-
3)).
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31
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77953871993
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Crystal data for complex 1: C84H136MgNa2O10, M, 1376.22, monoclinic, space group P2(1)/c, a, 23.0690(9) Å, b, 19.8537(8) Å, c, 20.7583(8) Å, α, 90.00, β, 115.221(2, γ, 90.00, V, 8601.1(6) Å3, T, 293(2) K, Z, 4, Dc, 1.063 g/cm3, F000, 3016, 2θmax, 26.29, 48786 reflections collected, 17124 unique (Rint, 0.0673, no. of observed reflections 7189 (I > 2σI, R1, 0.0676, wR2, 0.1607
-
2 = 0.1607.
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32
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31644446210
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Diekmann M., Bockstiegel G., Lützen A., Firedemann M., Saak W., Haase D., and Beckhaus R. Organometallics 25 (2006) 339
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Firedemann, M.4
Saak, W.5
Haase, D.6
Beckhaus, R.7
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33
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77953873332
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Crystal data for complex 2: C84H136MgK2O10, M, 1400.38, orthorhombic, space group Pbca, a, 20.2262(5) Å, b, 21.5029(5) Å, c, 41.5337(11) Å, α, 90.00, β, 90.00, γ, 90.00, V, 18063.9(8) Å3, T, 293(2) K, Z, 8, Dc, 0.983 g/cm3, F000, 5840, 2θmax, 26.46, 99295 reflections collected, 17963 unique (Rint, 0.1614, no. of observed reflections 4895 (I > 2σI, R1, 0.0652, wR2, 0.1495
-
2 = 0.1495.
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36
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0030243629
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Montaudo G., Montaudo M.S., Puglisi C., Samperi F., Spassky N., LeBorgne A., and Wisniewski M. Macromolecules 29 (1996) 6461
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0037167638
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