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_4313250
_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            'C44 H71 Cl3 Fe2 N16 O17.5'
_chemical_formula_weight         1322.22
_chemical_name_common            '[Fe2(O)(CH3COO)(N-MeIm)8](ClO4)3.2.5THF'
_chemical_name_systematic
;
  ?
;
_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                103.499(18)
_cell_angle_beta                 99.757(18)
_cell_angle_gamma                109.673(18)
_cell_formula_units_Z            2
_cell_length_a                   12.363(3)
_cell_length_b                   14.151(4)
_cell_length_c                   19.276(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      17.3
_cell_measurement_theta_min      4.5
_cell_volume                     2972.3(14)
_computing_cell_refinement       'Siemens P3/PC'
_computing_data_collection       'Siemens P3/PC'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL 6.1 (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL 6.1 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P3'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13650
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        2.7
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.8384
_exptl_absorpt_correction_T_min  0.7473
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2, Parkin, S., Moezzi, B. and Hope, H. J. Appl. Crystallogr. 28
(1995) 53-56.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         13650
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0706
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0963P)^2^+5.3105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.2044
_reflns_number_gt                9184
_reflns_number_total             13650
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0206140_5.cif
_cod_data_source_block           mn1224
_cod_original_cell_volume        2972.3(12)
_cod_original_formula_sum        'C44 H71 Cl3 Fe2 N16 O17.50'
_cod_database_code               4313250