Protonation/Reduction of Carbonyl-Rich Diiron Complexes and the Direct Observation of Triprotonated Species: Insights into the Electrocatalytic Mechanism of Hydrogen Formation
Liu, Yu-Chiao; Chu, Kai-Ti; Huang, Yi-Lan; Hsu, Cheng-Huey; Lee, Gene-Hsiang; Tseng, Mei-Chun; Chiang, Ming-Hsi; ACS Catalysis 6 (2016) 2559–; doi:10.1021/acscatal.5b02646

data_4513844
_publ_section_title
;
 Protonation/Reduction of Carbonyl-Rich Diiron Complexes and the Direct
 Observation of Triprotonated Species: Insights into the Electrocatalytic
 Mechanism of Hydrogen Formation
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              2559
_journal_paper_doi               10.1021/acscatal.5b02646
_journal_volume                  6
_journal_year                    2016
_chemical_formula_sum            'C33 H7 B Cl2 F20 Fe2 O6 S2'
_chemical_formula_weight         1136.92
_chemical_name_systematic
; 
 ? 
;
_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                 124.6992(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.9134(12)
_cell_length_b                   12.3868(7)
_cell_length_c                   17.2161(9)
_cell_measurement_reflns_used    6047
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.16
_cell_volume                     4017.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_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      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       '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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_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            15170
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_correction_T_min  0.6101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            orange-yelloW
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         9032
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                8269
_reflns_number_total             9032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs5b02646_si_004.cif
_cod_data_source_block           ic16884
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4513842--4513845.cif.
;
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4513844