Synthesis and Properties of Mono- and Dications of 1,1 -Diferrocen Yleth Ylenes

References

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• The crystallographic parameters of 6, 7, and 6+*I3 − were as follows: 6: C34H28Fe2, triclinic, Space group: P-1(No. 2), a = 9.950(2), b = 14.451(1), c = 9.745(2) Å, α = 106.17(1), β = 112.30(1), γ= 89.87(1)°, V = 1236.7(4) Å3 Z = 2, Dcalc = 1.472 g/cm3, Observed (F >s(F)): 4628, R 0.030, R w: 0.027; 7: C34H26Fe2, orthorhombic, Space group: Fdd2(No. 43), a = 18.247(7), b = 15.91(1), c = 16.835(8) Å,V = 4888(7) Å3 Z = 8, Dcalc = 1.484 g/cm3, Observed (F > s(F)): 1323, R: 0.023, R w: 0.016; 6+*I3 −: C34H28Fe2I3, monoclinic, Space group: P21/n(No. 14), a = 10.235(2), b = 10.271(3), c = 29.812(2) Å, β= 90.07(1)°, V = 3134.1(9) Å3 Z = 4, Dcalc = 1.969 g/cm3, Observed (F > s(F)): 3513, R: 0.046, R w 0.030.
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• Selected spectral data are as follows: 4: orange needles, mp 140–1 °C, 1H-NMR (400 MHz, CDCl3) δ= 4.30–4.28 (m, 4H), 4.20–4.17 (m, 4H), 4.01 (s, 10H), 2.12 (s, 6H); 13C-NMR (100 MHz, CDCls) δ= 133, 126, 90.5, 70.8, 69.1, 66.2, 24.6, MS (El) m/z = 424 (M+); Anal. Calcd for C24H24Fe2: C, 67.96%; H, 5.70%; Found: C, 67.50%; H, 5.80%. 5: orange crystals, mp 143–4 °C, 1H-NMR (400 MHz, CDC13) δ= 4.54–4.52 (m, 4H), 4.20–4.18 (m, 4H), 4.03 (s, 10H); 2.64–2.58 (m, 4H), 1.73–1.67 (m, 4H); 13C-NMR (100 MHz, CDCl3) 5= 144, 123, 89.5, 70.1, 69.1, 66.4, 35.0, 26.8; MS (El) m/z = 450 (M+); Anal. Calcd for C26H26Fe2: C, 69.37%; H, 5.82%; Found: C, 69.12%; H, 5.82%. 6: red crystals, mp = 250 °C (decomp.), H-NMR (400 MHz, CDC13) δ= 7.27–7.18 (m, 6H), 7.10–7.05 (m, 4H), 4.60–4.59 (m, 4H), 4.18–4.16 (m, 4H), 4.16 (s, 10H); 13C- NMR (100 MHz, CDC13) δ= 147, 140, 134, 131, 128, 126, 86.7, 71.7, 69.7, 67.7; MS (El) m/z = 548 (M+); Anal. Calcd for C34H28Fe2: C, 74.48%; H, 5.15%; Found: C, 74.02%; H, 4.88%. 7: purple crystals, mp 263 °C (decomp.), 1H-NMR (400 MHz, CDC13) δ= 7.73 (d, J = 7.4 Hz), 7.65 (d, J = 4.3 Hz, 2H), 7.24 (dd, J = 8.4, 7.4 Hz, 2H), 7.06 (dd, J = 8.4, 4.3 Hz, 2H), 4.68–4.44 (brs, 8H); 4.16 (s, lOH); 13C-NMR (100 MHz, CDC13) 5= 146, 141, 138, 133, 125, 125, 124, 119, 85.3, 71.1, 70.6, 70.1; MS (EI): m/z = 546 (M+); Anal. Calcd for C34H26Fe2: C, 74.76%; H, 4.80%; Found: C, 74.91%; H, 4.72%.
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