Synthesis and Spectroscopic Studies of Non-Heme Diiron(III) Species with a Terminal Hydroperoxide Ligand: Models for Hemerythrin
Tadashi J. Mizoguchi; Jane Kuzelka; Bernhard Spingler; Jennifer L. DuBois; Roman M. Davydov; Britt Hedman; Keith O. Hodgson; Stephen J. Lippard; Inorganic Chemistry 40 (2001) 4662–4673; doi:10.1021/ic010076b

data_4320165
_publ_section_title
;
 Synthesis and Spectroscopic Studies of Non-Heme Diiron(III) Species with
 a Terminal Hydroperoxide Ligand: Models for Hemerythrin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4662
_journal_page_last               4673
_journal_paper_doi               10.1021/ic010076b
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C65.25 H66 F6 Fe2 N4 O12.5 S2'
_chemical_formula_weight         1396.04
_chemical_name_common            '[Fe2(O)(Ph4DBA)(DPE)2(OTf)2].0.5THF.0.25C5H12'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.7320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3723(3)
_cell_length_b                   15.4576(4)
_cell_length_c                   33.65140(10)
_cell_measurement_temperature    188(2)
_cell_volume                     6855.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  '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  0.0814
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42671
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.791722
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2894
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.418
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.0033(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     914
_refine_ls_number_reflns         15982
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1540
_refine_ls_R_factor_gt           0.0923
_refine_ls_shift/su_max          0.330
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1371P)^2^+10.2609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2705
_reflns_number_gt                9368
_reflns_number_total             15982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010076b_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C65.25 H66 F6 Fe2 N4 O12.50 S2'
_cod_database_code               4320165