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_7717033
_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 H34 Cl Co N6 O6'
_chemical_formula_sum            'C46 H34 Cl Co N6 O6'
_chemical_formula_weight         861.17
_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                71.8550(10)
_cell_angle_beta                 83.2580(10)
_cell_angle_gamma                65.9430(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0461(5)
_cell_length_b                   13.7395(6)
_cell_length_c                   14.2433(6)
_cell_measurement_reflns_used    9518
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.57
_cell_volume                     2215.24(16)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27613
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.265
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.7123
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0500P)^2^+2.7142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6236
_reflns_number_total             7795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00650j2.cif
_cod_data_source_block           JK250_sq
_cod_depositor_comments
'Adding full bibliography for 7717032--7717034.cif.'
_cod_database_code               7717033
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3A(0.043) H4(0.065) H5(0.061) H6(0.061) H7(0.044) H10(0.031)
 H11(0.038) H12(0.038) H13(0.037) H14(0.03) H17(0.03) H18(0.036) H19(0.047)
 H20(0.055) H21(0.044) H24(0.027) H25(0.031) H26(0.033) H27(0.032) H28(0.028)
 H29(0.038) H30(0.043) H32(0.028) H33(0.027) H34A(0.034) H34B(0.034) H37(0.037)
 H38(0.042) H39(0.038) H41(0.036) H42(0.035) H43(0.03)
 Fixed X: H3A(0.478451) H4(0.387451) H5(0.274912) H6(0.25674) H7(0.347939)
 H10(0.452758) H11(0.31797) H12(0.136922) H13(0.092427) H14(0.227193)
 H17(0.662241) H18(0.748675) H19(0.920001) H20(1.007568) H21(0.924625)
 H24(0.807045) H25(0.945954) H26(1.084229) H27(1.080923) H28(0.939105)
 H29(0.433769) H30(0.28779) H32(0.371189) H33(0.513983) H34A(0.156128)
 H34B(0.246029) H37(-0.060456) H38(-0.142651) H39(-0.085724) H41(0.02965)
 H42(0.163586) H43(0.247733) H1(0.64987) H3(0.56556)
 Fixed Y: H3A(0.085667) H4(0.052881) H5(0.200288) H6(0.379723) H7(0.413853)
 H10(0.090067) H11(0.01955) H12(0.103854) H13(0.257634) H14(0.327818)
 H17(0.58297) H18(0.623378) H19(0.494273) H20(0.325222) H21(0.284133)
 H24(0.592725) H25(0.657127) H26(0.560487) H27(0.402137) H28(0.340576)
 H29(0.495285) H30(0.667031) H32(0.700854) H33(0.527058) H34A(0.815924)
 H34B(0.870904) H37(0.783217) H38(0.853928) H39(0.973754) H41(1.089974)
 H42(1.145388) H43(1.070462) H1(0.358941) H3(0.31499)
 Fixed Z: H3A(0.693617) H4(0.581469) H5(0.456184) H6(0.438702) H7(0.547694)
 H10(0.964191) H11(1.035985) H12(0.968714) H13(0.828738) H14(0.75432)
 H17(0.937944) H18(1.047212) H19(1.120572) H20(1.084672) H21(0.972853)
 H24(0.780631) H25(0.707184) H26(0.611499) H27(0.586309) H28(0.654661)
 H29(0.887077) H30(0.846875) H32(0.559518) H33(0.6065) H34A(0.71921)
 H34B(0.682054) H37(0.487549) H38(0.33065) H39(0.204124) H41(0.147155)
 H42(0.18243) H43(0.339204) H1(0.601221) H3(0.97932)
;
_shelx_res_checksum              27301
_shelx_hkl_checksum              80854
_shelx_fab_checksum              3214
_shelx_shelxl_version_number     2018/3