Mixed-Valent {FeIV(μ-O)(μ-carboxylato)2FeIII}3+ Core
Leonardo D. Slep; Ana Mijovilovich; Wolfram Meyer-Klaucke; Thomas Weyhermüller; Eckhard Bill; Eberhard Bothe; Frank Neese; Karl Wieghardt; Journal of the American Chemical Society 125 (2003) 15554–15570; doi:10.1021/ja030377f

data_4114476
_publ_section_title
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 Mixed-Valent {FeIV(\m-O)(\m-carboxylato)2FeIII}3+ Core
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15554
_journal_page_last               15570
_journal_paper_doi               10.1021/ja030377f
_journal_volume                  125
_journal_year                    2003
_chemical_formula_structural     '[C22H37BFe2N9O5]+,(PF6)-,0.5 MeCN,0.25 Et2O'
_chemical_formula_sum            'C24 H41 B F6 Fe2 N9.5 O5.25 P'
_chemical_formula_weight         814.14
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   32.721(4)
_cell_length_b                   49.518(5)
_cell_length_c                   8.6090(8)
_cell_measurement_reflns_used    6395
_cell_measurement_temperature    100(2)
_cell_volume                     13949(3)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w, 0.3 deg./frame'
_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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38686
_diffrn_reflns_theta_max         34.11
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   'SADABS, G.M. Sheldrick 1994'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             6712
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.086
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.033(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         12012
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_obs          0.0541
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+19.6201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1165
_refine_ls_wR_factor_obs         0.1063
_reflns_number_observed          8899
_reflns_number_total             12034
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja030377f.cif
_cod_data_source_block           4
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+19.6201P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+19.6201P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_formula_sum        'C24 H41 B F6 Fe2 N9.50 O5.25 P'
_cod_database_code               4114476