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_4337468
_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         'C43 H50 Fe O N10, 2(B F4), 4(C2 H3 N)'
_chemical_formula_sum            'C51 H62 B2 F8 Fe N14 O'
_chemical_formula_weight         1116.62
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9781(16)
_cell_length_b                   11.5551(8)
_cell_length_c                   19.5801(13)
_cell_measurement_reflns_used    19357
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.61
_cell_measurement_theta_min      2.21
_cell_volume                     5425.0(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            84107
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.9385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5165
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+12.9195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                4276
_reflns_number_total             5165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4019585_si_002.cif
_cod_data_source_block           17
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4337468