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_4320164
_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            'C71.5 H79 F3 Fe2 N4 O9 S'
_chemical_formula_weight         1339.15
_chemical_name_common            '[Fe2(OH)(Ph4DBA)(DPE)2(OTf)].1.5PhCH3'
_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                97.1060(10)
_cell_angle_beta                 96.2900(10)
_cell_angle_gamma                111.2940(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1852(2)
_cell_length_b                   14.6388(2)
_cell_length_c                   19.7878(3)
_cell_measurement_temperature    188(2)
_cell_volume                     3217.57(9)
_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      188(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_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  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20371
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.837457
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         14209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0680P)^2^+2.5138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                11469
_reflns_number_total             14209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010076b_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        3217.57(8)
_cod_original_formula_sum        'C71.50 H79 F3 Fe2 N4 O9 S'
_cod_database_code               4320164