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Single-crystal structure and refinement data for 1: C 22H26F6FeN4O6S 2, Mw=676.44, monoclinic, space group P21, a=9.184(1, b=28.648(3, c=10.614(1) Å, β=90.950(2)°, V= 2792.1(5) Å3, Z=4, ρcalcd=1.609 Mgm-3, MoKα radiation (λ= 0.71073 Å, μ=0.774 mm-1, T=173(2) K. A total of 12444 (Rint=0.0435) independent reflections with 2θ<27.50° were collected. The resulting parameters were refined to converge at R1=0.0438 (I>2θ) for 739 parameters on 12444 independent reflections wR 2=0.0971, Max./min. residual electron density 0.626/-0.487 eÅ-3; GOF=1.026. Single-crystal structure and refinement data for 2: C33H38Cl
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-3; GOF=1.061. Further experimental details are provided in the Supporting Information. CCDC-657096 (1), CCDC-657097 (2), and CCDC-657098 (3) contain 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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While this paper was being reviewed, the crystal structure of [Fe II{(S,S)-BPBP}(NCCH3)2](SbF 6)2, a complex closely related to 1, was reported M. S. Chen, M. C. White, Science 2007, 318, 783, In this work, the authors reported that this complex reacted with H2O 2 in the presence of acetic acid to generate an oxidant capable of hydroxylation of tertiary C-H bonds with predictable selectivity, which is quite a remarkable achievement
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2 in the presence of acetic acid to generate an oxidant capable of hydroxylation of tertiary C-H bonds with predictable selectivity, which is quite a remarkable achievement.
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