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_4113355
_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         'C27 H24 F6 Fe N6 O6 S2'
_chemical_formula_sum            'C27 H24 F6 Fe N6 O6 S2'
_chemical_formula_weight         762.49
_chemical_name_common            01160
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier synthesis'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.821(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.574(3)
_cell_length_b                   19.237(4)
_cell_length_c                   12.930(3)
_cell_measurement_reflns_used    2339
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.2
_cell_volume                     3123.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Siemens CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14533
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.704
_exptl_absorpt_correction_T_max  0.9458
_exptl_absorpt_correction_T_min  0.9078
_exptl_absorpt_correction_type   mulit-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5459
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+4.700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                3680
_reflns_number_total             5459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047667wsi20040430_010136.cif
_cod_data_source_block           01160
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'placed geometrically' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4113355