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- Crystal data for 2 at −70°C with Mo Kα radiation: a = 800.0 (1), b = 783.0 (1), c = 3417.1 (7) pm, β = 91.61 (1)°; monoclinic, P21/n; Z = 4, μ(Mo) = 0.93 cm−1; 1457 unique reflections with I ≥ 2.0 σ(I). The structure was solved by direct methods (MULTAN) and refined by full-matrix least-squares on |F|. C, F and N atoms were refined with anisotropic thermal parameters. All H atoms were idealized using a riding model. The largest residual electron density in the final difference Fourier map was 0.34 e/Å3 near C2. The data/parameter ratio was 5.56. The final R factors were R = 0.071 and Rw = 0.045.
- Crystal data for 3 at −147°C with Mo Kα radiation: a = 1867.4 (1), b = 1584.8 (1), c = 1661.3 (1) pm, β = 109.43 (1)°; monoclinic, P21/n; Z = 8; μ(Mo) = 1.07 cm−1; 3872 unique reflections with I ≥ 3.0 σ(I). The structure was solved by direct methods (MULTAN) and refined by full-matrix least-squares on |F|. C, F and N atoms were refined with anisotropic thermal parameters. All H atoms were idealized using a riding model. The largest residual electron density in the final difference Fourier map was 0.23 e/Å3 near H48''. The data/parameter ratio was 6.45. The final R factors were R = 0.045 and Rw = 0.041.
- The asymmetric unit of 3 contains two independent molecules. The structural parameters of only one of the two independent molecules are discussed, but the corresponding parameters for the second molecule in the asymmetric unit are shown in brackets throughout the discussion.
- Crystal data for 4 at −100°C with Mo Kα radiation: a = 1138.3 (3), b = 1506.6 (3), c = 1456.8 (4) pm, β = 100.94 (2)°; monoclinic, P21/n; Z = 4; μ(Mo) = 1.19 cm−1; 2830 unique reflections with I ≥ 3.0 σ(I). The structure was solved by direct methods (MULTAN) and refined by full-matrix least-squares on |F|. C, F and N atoms were refined with anisotropic thermal parameters. All H atoms were idealized using a riding model. The largest residual electron density in the final difference Fourier map was 0.21 e/Å3 near H4'. The data/parameter ratio was 8.70. The final R factors were R = 0.043 and Rw = 0.041.
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- Dixon, D. A.; Fukunaga, T.; Smart, B. E. J. Am. Chem. Soc. 1986, 108, 4027–4031.
- The original crystals of 8 that were submitted for X-ray diffraction studies were opaque and diffracted only weakly. After sitting in a vial for several days, smaller crystals grew in between the originals and the glass. The sample and adventitious water probably reacted with silicon in the glass causing it to lose a fluorine atom at C12, forming the double bond C12 = C11 and a SiF5− counterion (9). Crystal data for 9 at −115°C with Mo Kα radiation: a = 1128.5 (2), b = 1857.3 (3), c = 875.1 (1) pm, β = 112.24 (1)°; triclinic, P1; Z = 4; μ(Mo) = 2.60 cm−1; 2483 unique reflections with I ≥ 2.0 σ(I). The structure was solved by direct methods (SHELXS) and refined by full-matrix least-squares on |F|. C, F and N atoms were refined with anisotropic thermal parameters. All H atoms were idealized using a riding model. The Fourier map was 0.70 e/Å3. The data/parameter ratio was 5.10. The final R factors were R = 0.057 and Rw = 0.046. The crystals first submitted looked opaque.
- Crystal data for 13 at −100°C with Mo Kα radiation: a = 1492.5 (3), b = 1264.1 (2), c = 1726.0 (3) pm, β = 125.30 (1)°; monoclinic, P21/n; Z = 4; μ(Mo) = 1.32 cm−1; 3328 unique reflections with I ≥ 3.0 σ(I). The structure was solved by direct methods (MULTAN) and refined by full-matrix least-squares on |F|. C, F and N atoms were refined with anisotropic thermal parameters. All H atoms were idealized using a riding model. The Fourier map was 0.37 e/Å3. The data/parameter ratio was 7.53. The final R factors were R = 0.050 and Rw = 0.053. The asymmetric unit consists of one carbene derivative co-crystallized with one THF in general positions.
- Crystal data for 14 at −70°C with Mo Kα radiation: a = 3654.0 (8), b = 1322.4 (2), c = 2582.6 (8) pm; β = 101.96 (1)°;monoclinic, C2/c; Z = 8; μ(Mo) = 1.12 cm−1; 2718 unique reflections with I ≥ 3.0 σ(I). The structure was solved by direct methods (MULTAN) and refined by full-matrix least-squares on |F|. C, F and N atoms were refined with anisotropic thermal parameters. All H atoms were idealized with C-H = 0.95Å. The Fourier map was 0.22 e/Å3. The data/parameter ratio was 4.01. The final R factors were R = 0.047 and Rw = 0.035. The asymmetric unit consists of two carbene molecules co-crystallized with one half a THF molecule lying on the two-fold.