Structural Insights into Nonheme Alkylperoxoiron(III) and Oxoiron(IV) Intermediates by X-ray Absorption Spectroscopy
Jan-Uwe Rohde; Stéphane Torelli; Xiaopeng Shan; Mi Hee Lim; Eric J. Klinker; József Kaizer; Kui Chen; Wonwoo Nam; Lawrence Que; Journal of the American Chemical Society 126 (2004) 16750–16761; doi:10.1021/ja047667w

data_4113356
_publ_section_title
;
 Structural Insights into Nonheme Alkylperoxoiron(III) and Oxoiron(IV)
 Intermediates by X-ray Absorption Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16750
_journal_page_last               16761
_journal_paper_doi               10.1021/ja047667w
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety
'Fe N5 C28 H29 S O3 F3, S 03 c F3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C31 H34 F6 Fe N5 O6.5 S2'
_chemical_formula_weight         814.60
_chemical_name_common            'Benzyl Trispic Iron (II)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.651(12)
_cell_angle_beta                 100.815(13)
_cell_angle_gamma                109.097(12)
_cell_formula_units_Z            2
_cell_length_a                   9.209(6)
_cell_length_b                   13.755(10)
_cell_length_c                   15.137(11)
_cell_measurement_reflns_used    1611
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50.008
_cell_measurement_theta_min      4.624
_cell_volume                     1747(2)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker sMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11446
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.847055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.910
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+1.4106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                5128
_reflns_number_total             6138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047667wsi20040430_010151.cif
_cod_data_source_block           03050m
_cod_original_formula_sum        'C31 H34 F6 Fe N5 O6.50 S2'
_cod_database_code               4113356