Reaction of (μ-Oxo)diiron(III) Core with CO2 in N-Methylimidazole: Formation of Mono(μ-carboxylato)(μ-oxo)diiron(III) Complexes with N-Methylimidazole as Ligands
Dana S. Marlin; Marilyn M. Olmstead; Pradip K. Mascharak; Inorganic Chemistry 42 (2003) 1681–1687; doi:10.1021/ic0206140

data_4313249
_publ_section_title
;
 Reaction of (\m-Oxo)diiron(III) Core with CO2 in N-Methylimidazole:
 Formation of Mono(\m-carboxylato)(\m-oxo)diiron(III) Complexes with
 N-Methylimidazole as Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1681
_journal_page_last               1687
_journal_paper_doi               10.1021/ic0206140
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C48 H76 Cl4 Fe2 N20 O19'
_chemical_formula_weight         1490.79
_chemical_name_common            '[Fe2(O)(N-MeIm)10](ClO4)4.2THF'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.060(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5262(14)
_cell_length_b                   17.0491(15)
_cell_length_c                   28.578(3)
_cell_measurement_reflns_used    968
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      2.4
_cell_volume                     6590.4(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      92(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_sigmaI/netI    0.061
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            62854
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     'seven reflections omitted'
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         15046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1122P)^2^+10.3401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                9633
_reflns_number_total             15046
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0206140_4.cif
_cod_data_source_block           mn1223
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4313249