Chlorocobaloxime containing <i>N</i>-(4-pyridylmethyl)-1,8-naphthalamide peripheral ligands: synthesis, characterization and enhanced electrochemical hydrogen evolution in alkaline medium.
Kumar Yadav, Jitendra; Singh, Baghendra; Pal, Sarvesh Kumar; Singh, Nanhai; Lama, Prem; Indra, Arindam; Kumar, Kamlesh; Dalton transactions (Cambridge, England : 2003) 52 (2023) 936–946; doi:10.1039/d2dt02511f

data_7711943
_publ_section_title
;
 Chlorocobaloxime containing <i>N</i>-(4-pyridylmethyl)-1,8-naphthalamide
 peripheral ligands: synthesis, characterization and enhanced
 electrochemical hydrogen evolution in alkaline medium.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              936
_journal_page_last               946
_journal_paper_doi               10.1039/d2dt02511f
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C26 H25 Br Cl Co N6 O6'
_chemical_formula_sum            'C26 H25 Br Cl Co N6 O6'
_chemical_formula_weight         691.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-01 deposited with the CCDC.	2022-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.5130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1696(4)
_cell_length_b                   14.6019(6)
_cell_length_c                   21.0020(8)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.29
_cell_volume                     2755.5(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44173
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.294
_diffrn_reflns_theta_min         2.662
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.5425
_refine_diff_density_max         0.836
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+5.8848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6027
_reflns_number_total             6822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02511f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7711942--7711943.cif.'
_cod_database_code               7711943
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.652
_olex2_refinement_description
;
1. Others
 Sof(Br1B)=Sof(C16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=
 Sof(H19B)=Sof(C20B)=Sof(C21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=
 Sof(C24B)=Sof(C25B)=1-FVAR(1)
 Sof(Br1A)=Sof(C16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(C20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=
 Sof(C24A)=Sof(C25A)=FVAR(1)
 Fixed Uiso: C24B(0.021)
 Fixed X: H1O(0.521351) H3O(0.08591)
 Fixed Y: H1O(0.33804) H3O(0.41825)
 Fixed Z: H1O(0.58814) H3O(0.71433)
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C12(H12), C13(H13), C17A(H17A), C18A(H18A), C21A(H21A),
 C22A(H22A), C23A(H23A), C17B(H17B), C18B(H18B), C19B(H19B), C22B(H22B),
 C23B(H23B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              93687
_shelx_hkl_checksum              63933
_olex2_submission_special_instructions 'No special instructions were received'