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For the simultaneous formation of boronic esters and imines in the coordination sphere of boron see reference [5b,f] and: a A. M. Kelly, Y. Pérez-Fuertes, S. Arimori, S. D. Bull, T. D. James, Org. Lett. 2006, 8, 1971-1974;
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53549117974
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Crystal data for 1·2CHCl3: C52H 46B4Cl6N4O8, Mr, 1110.87, monoclinic, space group P2 1/n, a, 6.475(3, b, 19.32(2, c, 21.19(2) Å, β, 94.73(6)°, V, 2641(4) Å3, Z, 2, ρcalcd, 1.397 gcm-3, μ, 0.383 mm-1, F(000, 1144, crystal dimensions 0.62 × 0.09 × 0.08 mm3, T, 100(2) K, MoKα radiation, λ, 0.71073 Å, θ, 3.31-22.99°, 7 ≤ h ≤ 7, 21≤ k ≤ 21, 23 ≤ l ≤ 23, 25326 reflections collected, 3606 independent reflections, Rint, 0.2049, R1, 0.1103 [I > 2σ(I, wR2, 0.2643 all data, largest difference peak 0.384 e Å-3, largest difference minimu
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-3. Structure solution and refinement by SHELX97 (G. M. Sheldrick, SHELX97, Programs for Crystal Structure Analysis, University of GMttingen, GMttingen (Germany), 1998). Hydrogen atoms were placed in calculated positions using the riding model. CCDC-667829 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
-
-
-
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47
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53549132771
-
-
Crystal data for 2·4CHCl3: C73H 82B6Cl12N8O12, Mr, 1753.73, rhombohedral, space group R3c, a, 18.110(3, b, 18.110(3, c, 50.971(10) Å, V, 14477(4) Å3, Z, 6, ρcalcd, 1.207 gcm-3, m, 0.398 mm-1, F(000, 5436, crystal dimensions 0.33 × 0.33 × 0.21 mm3, T, 100(2) K, MoKα radiation, λ, 0.71073 Å, θ, 3.45-20.06°, 17 ≤ h ≤ 17, 7 ≤ k ≤ 17, 48 ≤ l ≤ 48, 36 623 reflections collected, 1514 independent reflections, Rint, 0.1511, R1, 0.1298 [I > 2σ(I, wR2, 0.3347 all data, largest difference peak 0.496 e Å-3, largest difference minimum -0.318 eÅ-3
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1 value because of the extremely weak diffraction of the sample, though the crystal was not small. Diffraction data have been measured up to 20.06°, but this prevented us from collecting enough reflections for an acceptable refinement of the structure. However, the connectivity is clear, and the disordered solvent (an important part of the structure) is well defined. CCDC-671424 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/ data_request/cif.
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53549117426
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Crystal data for 4·3C2H4Cl 2: C70H60B4Br2Cl 10N8O14Re2, Mr, 2167.22, triclinic, space group P1, a, 15.23(2, b, 16.991(12, c, 20.60(2) Å, α, 97.48(7, β, 107.74(9, γ, 101.23(8)°, V, 4876(9) Å3, Z, 2, ρcalcd, 1.476 gcm-3, μ, 3.628 mm-1, F(000, 2116, crystal dimensions 0.61 × 0.33 × 0.14 mm 3, T, 100(2) K, MoKα radiation, λ, 0.71073 Å, θ, 3.31-22.99°, 16 ≤ h ≤ 16, 18 ≤ k ≤ 18, 22 ≤ l ≤ 22, 55052 reflections collected, 13133 independent reflections, Rint, 0.1471, R1, 0.1079 [I > 2σ(I, wR2, 0.3088 al
-
-3. Structure solution and refinement by SHELX97 (G. M. Sheldrick, SHELX97, Programs for Crystal Structure Analysis, University of Göttingen, Göttingen (Germany), 1998). Hydrogen atoms were placed in calculated positions using the riding model. CCDC-667830 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
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0009779057
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53549135439
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The two crystallographically independent complexes show Re⋯Re distances of 23.8 and 24.1 Å, respectively.
-
The two crystallographically independent complexes show Re⋯Re distances of 23.8 and 24.1 Å, respectively.
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