Electrocatalytic hydrogen production by dinuclear cobalt(II) compounds containing redox-active diamidate ligands: a combined experimental and theoretical study.
Papanikolaou, Michael G.; Elliott, Alexander; McAllister, James; Gallos, John K.; Keramidas, Anastasios D.; Kabanos, Themistoklis A.; Sproules, Stephen; Miras, Haralampos N.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15718–15730; doi:10.1039/d0dt02617d

data_7706249
_publ_section_title
;
 Electrocatalytic hydrogen production by dinuclear cobalt(II) compounds
 containing redox-active diamidate ligands: a combined experimental and
 theoretical study.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15718
_journal_page_last               15730
_journal_paper_doi               10.1039/d0dt02617d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C50 H30 Co2 N10 O4, 2(C HCl3) [+ solvent]'
_chemical_formula_sum            'C52 H32 Cl6 Co2 N10 O4'
_chemical_formula_weight         1191.43
_space_group_crystal_system      hexagonal
_space_group_IT_number           172
_space_group_name_Hall           'P 64'
_space_group_name_H-M_alt        'P 64'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-13 deposited with the CCDC.	2020-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   18.412(3)
_cell_length_b                   18.412(3)
_cell_length_c                   13.362(3)
_cell_measurement_reflns_used    3180
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.679
_cell_measurement_theta_min      2.210
_cell_volume                     3922.9(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Apex II Quazar CCD'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1317
_diffrn_reflns_av_unetI/netI     0.1471
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33616
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.480
_diffrn_reflns_theta_min         1.989
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.7376
_exptl_absorpt_correction_T_min  0.6402
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             1806
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 1130 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5245
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0163P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                3181
_reflns_number_total             5245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02617d2.cif
_cod_data_source_block           Compound_1
_cod_original_cell_volume        3922.8(18)
_cod_database_code               7706249
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.916
_shelx_res_checksum              11721
_shelx_fab_checksum              14269