Speciation of Ferric Phenoxide Intermediates during the Reduction of Iron(III)-μ-Oxo Dimers by Hydroquinone.
Kerber, William D.; Perez, Kaitlyn A.; Ren, Chuqiao; Siegler, Maxime A.; Inorganic chemistry 53 (2014) 11507–11516; doi:10.1021/ic5014347

data_4341315
_publ_section_title
;
 Speciation of Ferric Phenoxide Intermediates during the Reduction of
 Iron(III)-\m-Oxo Dimers by Hydroquinone.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11507
_journal_page_last               11516
_journal_paper_doi               10.1021/ic5014347
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H28 Fe N4 O2, Cl O4'
_chemical_formula_sum            'C29 H28 Cl Fe N4 O6'
_chemical_formula_weight         619.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.4308(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2646(2)
_cell_length_b                   15.2234(3)
_cell_length_c                   13.7942(3)
_cell_measurement_reflns_used    10032
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.94
_cell_measurement_theta_min      3.18
_cell_volume                     2785.42(9)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24135
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.885
_diffrn_reflns_theta_min         3.204
_exptl_absorpt_coefficient_mu    5.655
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.262
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       'long lath'
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 3519 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         9907
_refine_ls_number_restraints     962
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1110P)^2^+1.3184P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    0.816
_reflns_Friedel_fraction_max     0.803
_reflns_number_gt                9216
_reflns_number_total             9907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5014347_si_002.cif
_cod_data_source_block           6
_cod_depositor_comments          'Adding full bibliography for 4341315.cif.'
_cod_database_code               4341315
_shelxl_version_number           2013-2
_shelx_res_checksum              88142
_shelx_hkl_checksum              6292