Reduction of CO2 to CO Using Low-Coordinate Iron: Formation of a Four-Coordinate Iron Dicarbonyl Complex and a Bridging Carbonate Complex
Azwana R. Sadique; William W. Brennessel; Patrick L. Holland; Inorganic Chemistry 47 (2008) 784–786; doi:10.1021/ic701914m

data_4304410
_publ_section_title
;
Reduction of CO2 to CO Using Low-Coordinate Iron: Formation of a
Four-Coordinate Iron Dicarbonyl Complex and a Bridging Carbonate Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              784
_journal_page_last               786
_journal_paper_doi               10.1021/ic701914m
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C71 H106 Fe2 N4 O3'
_chemical_formula_sum            'C71 H106 Fe2 N4 O3'
_chemical_formula_weight         1175.30
_chemical_name_common            holas20
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 114.930(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.078(3)
_cell_length_b                   28.685(4)
_cell_length_c                   24.363(4)
_cell_measurement_reflns_used    3980
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.99
_cell_measurement_theta_min      2.38
_cell_volume                     13358(3)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            119705
_diffrn_reflns_theta_full        32.58
_diffrn_reflns_theta_max         32.58
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.8612
_exptl_absorpt_correction_T_min  0.8382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5088
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
'Flack H D (1983), 23097 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.448(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1498
_refine_ls_number_reflns         47203
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0854
_reflns_number_gt                40946
_reflns_number_total             47203
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701914m-file002_2.cif
_cod_data_source_block           2
_cod_database_code               4304410