Axial ligand-induced high electrocatalytic hydrogen evolution activity of molecular cobaloximes in homo- and heterogeneous medium.
Yadav, Jitendra Kumar; Singh, Baghendra; Mishra, Anjali; Pal, Sarvesh Kumar; Singh, Nanhai; Lama, Prem; Indra, Arindam; Kumar, Kamlesh; Dalton transactions (Cambridge, England : 2003) 53 (2024) 16747–16758; doi:10.1039/d4dt00650j

data_7717032
_publ_section_title
;
 Axial ligand-induced high electrocatalytic hydrogen evolution activity of
 molecular cobaloximes in homo- and heterogeneous medium.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16747
_journal_page_last               16758
_journal_paper_doi               10.1039/d4dt00650j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C46 H33 Br Cl Co N6 O6'
_chemical_formula_sum            'C46 H33 Br Cl Co N6 O6'
_chemical_formula_weight         940.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-04-08
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2023-05-16 deposited with the CCDC.	2024-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                71.891(3)
_cell_angle_beta                 84.233(3)
_cell_angle_gamma                65.507(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6333(12)
_cell_length_b                   13.9675(15)
_cell_length_c                   14.1353(15)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.37
_cell_volume                     2156.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-2013 (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-III detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            44226
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.389
_diffrn_reflns_theta_min         2.893
_exptl_absorpt_coefficient_mu    1.442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   0.7455
_exptl_transmission_factor_min   0.6744
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         9765
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+3.5846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7660
_reflns_number_total             9765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00650j2.cif
_cod_data_source_block           JK245_sq
_cod_depositor_comments
'Adding full bibliography for 7717032--7717034.cif.'
_cod_database_code               7717032
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3A(0.06) H4(0.09) H5(0.076) H6(0.057) H7(0.042) H10(0.034)
 H11(0.04) H12(0.04) H13(0.038) H14(0.035) H17(0.037) H18(0.044) H19(0.052)
 H20(0.061) H21(0.045) H24(0.034) H25(0.041) H26(0.047) H27(0.042) H28(0.036)
 H29(0.032) H30(0.037) H32(0.04) H33(0.032) H34A(0.068) H34B(0.068) H37A(0.034)
 H38A(0.041) H43A(0.038) H44A(0.045) H45A(0.048) H37B(0.038) H38B(0.038)
 H39B(0.022) H43B(0.034) H44B(0.018)
 Fixed X: H3A(0.491833) H4(0.403996) H5(0.29006) H6(0.27692) H7(0.368926)
 H10(0.464972) H11(0.330379) H12(0.153151) H13(0.109729) H14(0.245325)
 H17(0.661154) H18(0.731125) H19(0.910365) H20(1.024892) H21(0.959619)
 H24(0.817564) H25(0.950208) H26(1.094457) H27(1.104407) H28(0.969625)
 H29(0.446675) H30(0.300546) H32(0.394219) H33(0.53457) H34A(0.171801)
 H34B(0.269257) H37A(-0.053383) H38A(-0.13357) H43A(0.298152) H44A(0.218766)
 H45A(0.077015) H37B(-0.058734) H38B(-0.173041) H39B(-0.124357) H43B(0.224636)
 H44B(0.10964) H3O(0.58239) H1O(0.68259)
 Fixed Y: H3A(0.078606) H4(0.050017) H5(0.198766) H6(0.375467) H7(0.404107)
 H10(0.103362) H11(0.029568) H12(0.09001) H13(0.227177) H14(0.300162)
 H17(0.575494) H18(0.624785) H19(0.507811) H20(0.348241) H21(0.302733)
 H24(0.594061) H25(0.666526) H26(0.573884) H27(0.41011) H28(0.33877)
 H29(0.486895) H30(0.661879) H32(0.69275) H33(0.514623) H34A(0.813618)
 H34B(0.861461) H37A(0.820271) H38A(0.914774) H43A(1.064946) H44A(1.163184)
 H45A(1.122893) H37B(0.772801) H38B(0.834906) H39B(0.940522) H43B(1.068366)
 H44B(1.150947) H3O(0.31751) H1O(0.328691)
 Fixed Z: H3A(0.701771) H4(0.58052) H5(0.45207) H6(0.433695) H7(0.550671)
 H10(0.990665) H11(1.06157) H12(0.977852) H13(0.825552) H14(0.752287)
 H17(0.941908) H18(1.057842) H19(1.138707) H20(1.097059) H21(0.975089)
 H24(0.774278) H25(0.694238) H26(0.598286) H27(0.581681) H28(0.657632)
 H29(0.888431) H30(0.8436) H32(0.557754) H33(0.60868) H34A(0.71422)
 H34B(0.681459) H37A(0.443843) H38A(0.285096) H43A(0.366211) H44A(0.199508)
 H45A(0.150433) H37B(0.523733) H38B(0.379469) H39B(0.228562) H43B(0.310518)
 H44B(0.146955) H3O(0.98388) H1O(0.618501)
;
_shelx_res_checksum              9695
_shelx_hkl_checksum              39230
_shelx_fab_checksum              4140
_shelx_shelxl_version_number     2018/3