Directing the Reactivity of [HFe4N(CO)12]- toward H+ or CO2 Reduction by Understanding the Electrocatalytic Mechanism
M. Diego Rail; Louise A. Berben; Journal of the American Chemical Society 133 (2011) 18577–18579; doi:10.1021/ja208312t

data_4107139
_publ_section_title
;
 Directing the Reactivity of [HFe4N(CO)12]- toward H+ or CO2 Reduction by
 Understanding the Electrocatalytic Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18577
_journal_page_last               18579
_journal_paper_doi               10.1021/ja208312t
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C20 H20 Fe4 N2 O12'
_chemical_formula_weight         703.78
_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                107.847(2)
_cell_angle_beta                 94.415(2)
_cell_angle_gamma                100.224(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1358(8)
_cell_length_b                   12.1565(11)
_cell_length_c                   12.4654(11)
_cell_measurement_reflns_used    5998
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.29
_cell_volume                     1284.0(2)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15674
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    2.279
_exptl_absorpt_correction_T_max  0.7716
_exptl_absorpt_correction_T_min  0.6845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_description       Block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+3.5701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                5492
_reflns_number_total             7182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208312t_si_002.cif
_cod_data_source_block           es27
_cod_database_code               4107139