Enzyme-Inspired Synthetic Proton Relays Generate Fast and Acid-Stable Cobalt-Based H2 Production Electrocatalysts
Dolui, Dependu; Khandelwal, Shikha; Shaik, Althaf; Gaat, Deepika; Thiruvenkatam, Vijay; Dutta, Arnab; ACS Catalysis  (2019) 10115–; doi:10.1021/acscatal.9b02953

data_4514903
_publ_section_title
;
 Enzyme-Inspired Synthetic Proton Relays Generate Fast and Acid-Stable
 Cobalt-Based H2 Production Electrocatalysts
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              10115
_journal_paper_doi               10.1021/acscatal.9b02953
_journal_year                    2019
_chemical_formula_sum            'C22 H35 Cl2 Co N6 O7.5'
_chemical_formula_weight         633.39
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                63.668(5)
_cell_angle_beta                 88.605(7)
_cell_angle_gamma                74.638(6)
_cell_formula_units_Z            4
_cell_length_a                   13.559(2)
_cell_length_b                   15.380(2)
_cell_length_c                   15.989(3)
_cell_measurement_reflns_used    9745
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.23
_cell_volume                     2864.8(8)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            77427
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         2.232
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012/1)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.055
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.033(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1437
_refine_ls_number_reflns         28211
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+3.1264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                24334
_reflns_number_total             28211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b02953_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C88 H140 Cl8 Co4 N24 O30'
_cod_original_formula_weight         2533.56
_cod_original_formula_units_Z            1
_cod_database_code               4514903
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              55552
_shelx_hkl_checksum              43730