Regioselectivity in ligand substitution reactions on diiron complexes governed by nucleophilic and electrophilic ligand properties.
Bethel, Ryan D.; Crouthers, Danielle J.; Hsieh, Chung-Hung; Denny, Jason A.; Hall, Michael B.; Darensbourg, Marcetta Y.; Inorganic chemistry 54 (2015) 3523–3535; doi:10.1021/acs.inorgchem.5b00072

data_4346027
_publ_section_title
;
 Regioselectivity in ligand substitution reactions on diiron complexes
 governed by nucleophilic and electrophilic ligand properties.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3523
_journal_page_last               3535
_journal_paper_doi               10.1021/acs.inorgchem.5b00072
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
'C14 H23 Fe2 N3 O4 P S2, B F4, 2/3(C H2 Cl2)'
_chemical_formula_sum       'C14.66667 H24.33333 B Cl1.33333 F4 Fe2 N3 O4 P S2'
_chemical_formula_weight         647.57
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                85.662(3)
_cell_angle_beta                 65.355(3)
_cell_angle_gamma                78.491(3)
_cell_formula_units_Z            6
_cell_length_a                   15.5833(10)
_cell_length_b                   15.8471(10)
_cell_length_c                   17.7406(11)
_cell_measurement_temperature    110(2)
_cell_volume                     3901.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and gamma 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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            161256
_diffrn_reflns_theta_full        32.96
_diffrn_reflns_theta_max         32.96
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.452
_refine_diff_density_min         -1.911
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         28984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.520
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+6.3131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1696
_reflns_number_gt                20567
_reflns_number_total             28984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00072_si_002.cif
_cod_data_source_block           4-IMe
_cod_depositor_comments
;

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C44 H73 B3 Cl4 F12 Fe6 N9 O12 P3 S6'
_cod_original_formula_weight         1942.71
_cod_original_formula_moiety
'3(C14 H23 Fe2 N3 O4 P S2), 3(B F4), 2(C H2 Cl2)'
_cod_original_formula_units_Z            2
_cod_database_code               4346027