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Hints to the viability can be derived from previous investigations in which diethyl malonate derivates coordinated to iron(II) centers were unselectively oxygenated and cleaved by dioxygen,[8] and from work by Que et al, in which the reaction of an α keto acid-iron(II) compound with dioxygen led to partial C-C bond cleavage adjacent to the carbonyl group.[9
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X-ray structure analysis of 1: C28H 37BFeN6O4, Mr=588.30, monoclinic, P21/c, a=9.8480(4, b=19.0788(8, c= 16.2832(6) Å, β=101.146(3)°, V=3001.7(2) Å3, Z=4, T= 100(2) K, F 000=1240, μ=0.545 mm-1, Θ=2.55-29.00°, reflections collected 30965, independent reflections 7909 (R int= 0.0373, GoF=0.992, R1=0.0297, wR 2=0.0709, largest diffraction peak/hole 0.348/-0.300 eÅ-3. The crystal was mounted on a glass fiber and then transferred into the cold nitrogen gas stream of the diffractometer (Stoe IPDS2N, MoKα radiation, λ= 0.71073 Å. The structure was solved by direct methods (SHELXS-97, 20] refined versus F2 (SHELXL-97)[21] with anisotropic tem
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[21] with anisotropic temperature factors for all non-hydrogen atoms. All hydrogen atoms were added geometrically and refined by using a riding model. CCDC-692202 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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37049096497
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54749148007
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4 instead of 3M HCl. It had been confirmed beforehand that this modification of the workup procedure has no influence on the result of the product analysis.
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4 instead of 3M HCl. It had been confirmed beforehand that this modification of the workup procedure has no influence on the result of the product analysis.
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54749096439
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G. M. SHELXS-97, Program for Crystal Structure Solution, University of Göttingen 1997.
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G. M. SHELXS-97, Program for Crystal Structure Solution, University of Göttingen 1997.
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54749117483
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G. M. SHELXL-97, Sheldrick, Program for Crystal Structure Refinement, University of Göttingen 1997.
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G. M. SHELXL-97, Sheldrick, Program for Crystal Structure Refinement, University of Göttingen 1997.
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