Electroreduction of a CoIIcoordination complex producing a metal‒organic film with high performance toward electrocatalytic hydrogen evolution
Bezerra, Leticia S.; Rosa, Persiely P.; Fortunato, Guilherme V.; Pizzuti, Lucas; Casagrande, Gleison A.; Maia, Gilberto; Journal of Materials Chemistry A 6 (2018) 19590–; doi:10.1039/C8TA07340F

data_7237198
_publ_section_title
;
 Electroreduction of a CoIIcoordination complex producing a metal--organic
 film with high performance toward electrocatalytic hydrogen evolution
;
_journal_issue                   40
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              19590
_journal_paper_doi               10.1039/C8TA07340F
_journal_volume                  6
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_compound_source        syntetic
_chemical_formula_moiety         'C34 H34 Cl2 Co N6 O2 S2'
_chemical_formula_sum            'C34 H34 Cl2 Co N6 O2 S2'
_chemical_formula_weight         752.62
_chemical_melting_point          476
_chemical_name_common            'Pyrazoline Co(II) complex'
_chemical_name_systematic        'bis(thiocabamoylpirazoline)Co(II) Chloride'
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2016-07-18T14:55:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-10-23 deposited with the CCDC.
2018-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   30.9254(9)
_cell_length_b                   30.9254(9)
_cell_length_c                   19.3130(14)
_cell_measurement_reflns_used    6059
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      1.32
_cell_measurement_wavelength     0.71073
_cell_volume                     15996.0(13)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38635
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.405
_diffrn_reflns_theta_min         1.317
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.79
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Neddle
_exptl_crystal_F_000             7002
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone and Dichlorometane'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.05
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6059
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+12.5601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3378
_reflns_number_total             6059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta07340f2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        15996.0(15)
_cod_original_sg_symbol_H-M      'R 3 c '
_cod_database_code               7237198
_shelx_estimated_absorpt_t_min   0.815
_shelx_estimated_absorpt_t_max   0.992