Versatile reactivity of a solvent-coordinated diiron(II) compound: synthesis and dioxygen reactivity of a mixed-valent Fe(II)Fe(III) species.
Majumdar, Amit; Apfel, Ulf-Peter; Jiang, Yunbo; Moënne-Loccoz, Pierre; Lippard, Stephen J.; Inorganic chemistry 53 (2014) 167–181; doi:10.1021/ic4019585

data_4337462
_publ_section_title
;
 Versatile reactivity of a solvent-coordinated diiron(II) compound:
 synthesis and dioxygen reactivity of a mixed-valent Fe(II)Fe(III)
 species.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              167
_journal_page_last               181
_journal_paper_doi               10.1021/ic4019585
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C63 H64 Fe2 N10 O3, 2(B F4), 2(C3 H7 N O)'
_chemical_formula_sum            'C69 H78 B2 F8 Fe2 N12 O5'
_chemical_formula_weight         1440.75
_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                98.098(2)
_cell_angle_beta                 95.663(2)
_cell_angle_gamma                101.203(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1498(16)
_cell_length_b                   16.280(2)
_cell_length_c                   17.653(2)
_cell_measurement_reflns_used    23225
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.20
_cell_volume                     3362.4(7)
_computing_cell_refinement       'SAINT 7.46A (Bruker-Axs,2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-Axs,2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-Axs,2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53875
_diffrn_reflns_theta_full        25.73
_diffrn_reflns_theta_max         25.73
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_correction_T_min  0.8865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.862
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         12706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0468P)^2^+5.0136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                10742
_reflns_number_total             12706
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4019585_si_002.cif
_cod_data_source_block           23
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3362.3(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4337462