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_4337469
_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         'C45 H53 Fe2 N11 O2, C3 H7 N O, 2(B F4)'
_chemical_formula_sum            'C48 H60 B2 F8 Fe2 N12 O3'
_chemical_formula_weight         1138.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.122(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8788(12)
_cell_length_b                   23.342(2)
_cell_length_c                   15.9680(14)
_cell_measurement_reflns_used    17184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.17
_cell_volume                     5133.1(8)
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            83460
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.9745
_exptl_absorpt_correction_T_min  0.9262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Sheldrick,2009)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         9751
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0912
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+23.7806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2200
_refine_ls_wR_factor_ref         0.2335
_reflns_number_gt                7865
_reflns_number_total             9751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4019585_si_002.cif
_cod_data_source_block           26
_cod_original_cell_volume        5133.0(8)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4337469