Mechanism of the electrocatalytic reduction of protons with diaryldithiolene cobalt complexes.
Letko, Christopher S.; Panetier, Julien A.; Head-Gordon, Martin; Tilley, T. Don; Journal of the American Chemical Society 136 (2014) 9364–9376; doi:10.1021/ja5019755

data_4122070
_publ_section_title
;
 Mechanism of the electrocatalytic reduction of protons with
 diaryldithiolene cobalt complexes.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9364
_journal_page_last               9376
_journal_paper_doi               10.1021/ja5019755
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C28 H16 Co F4 S4, 2(C16 H36 N)'
_chemical_formula_sum            'C60 H88 Co F4 N2 S4'
_chemical_formula_weight         1100.49
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2013-08-11
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                85.314(2)
_cell_angle_beta                 87.963(2)
_cell_angle_gamma                77.283(2)
_cell_formula_units_Z            1
_cell_length_a                   8.1573(3)
_cell_length_b                   13.8820(5)
_cell_length_c                   14.4088(5)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.4267
_cell_measurement_theta_min      2.8373
_cell_volume                     1586.04(10)
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_molecular_graphics    WINGX
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1165
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19825
_diffrn_reflns_theta_full        25.43
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         1.42
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_correction_T_min  0.9155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             589
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0575P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                4841
_reflns_number_total             5791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5019755_si_002.cif
_cod_data_source_block           '[NBu4]2[1F]'
_cod_depositor_comments
'Adding full bibliography for 4122065--4122071.cif.'
_cod_database_code               4122070
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B),
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C28(H28A,H28B), C30(H30A,H30B),
  C31(H31A,H31B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C18(H18), C26(H26), C27(H27), C29(H29), C32(H32), C34(H34)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C)
;