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_4313247
_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_moiety         Fe2C34H51N16O4,C4H8O,0.5(C4H6N2),3(ClO4)
_chemical_formula_sum            'C40 H62 Cl3 Fe2 N17 O17'
_chemical_formula_weight         1271.12
_chemical_name_common            '[Fe2O(O2COCH3)(N-MeIm)8](ClO4)3.0.5NMeIm.THF'
_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                89.336(4)
_cell_angle_beta                 82.316(4)
_cell_angle_gamma                77.390(4)
_cell_formula_units_Z            2
_cell_length_a                   13.0447(9)
_cell_length_b                   13.5509(9)
_cell_length_c                   18.4953(14)
_cell_measurement_reflns_used    4645
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.1
_cell_volume                     3161.3(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.038
_diffrn_reflns_av_sigmaI/netI    0.064
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28693
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.9371
_exptl_absorpt_correction_T_min  0.7518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.518
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.0033(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     726
_refine_ls_number_reflns         11695
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2886
_refine_ls_wR_factor_ref         0.3263
_reflns_number_gt                7574
_reflns_number_total             11695
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic0206140_2.cif
_cod_data_source_block           mn1205
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313247