Design and synthesis of dinuclear cobalt(ii) complexes derived from strong π-acidic ligands: crystal structure and studies on the oxidation of sp3 C–H bonds
Singh, Anshu; Boro, Bishal; Maji, Ankur; Singh, Ovender; Singh, Sain; Singh, Udai P.; Ghosh, Kaushik; New Journal of Chemistry 47 (2023) 8951–8959; doi:10.1039/D3NJ00128H

data_7062402
_publ_section_title
;
 Design and synthesis of dinuclear cobalt(ii) complexes derived from
 strong \p-acidic ligands: crystal structure and studies on the oxidation
 of sp3 C--H bonds
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8951
_journal_page_last               8959
_journal_paper_doi               10.1039/D3NJ00128H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C26 H28 Cl4 Co2 N6 O2'
_chemical_formula_sum            'C26 H28 Cl4 Co2 N6 O2'
_chemical_formula_weight         716.20
_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
_audit_creation_date             2023-03-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-03-29 deposited with the CCDC.	2023-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                65.8370(10)
_cell_angle_beta                 70.6870(10)
_cell_angle_gamma                89.6210(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1270(3)
_cell_length_b                   9.5751(3)
_cell_length_c                   9.8287(3)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.60
_cell_measurement_theta_min      2.36
_cell_volume                     731.27(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.983
_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  0.0299
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36244
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.624
_diffrn_reflns_theta_min         2.358
_exptl_absorpt_coefficient_mu    1.536
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0968 before and 0.0413 after correction.
The Ratio of minimum to maximum transmission is 0.9240.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       block
_exptl_crystal_F_000             364.0
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.021
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4426
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0377P)^2^+0.2527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4151
_reflns_number_total             4500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00128h2.cif
_cod_data_source_block           kg_sr_01_0088_0m
_cod_depositor_comments          'Adding full bibliography for 7062402.cif.'
_cod_database_code               7062402
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.773
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1A-H1A
 0.87 with sigma of 0.01
 Co1A-H1A
 2.643898 with sigma of 0.02
 C13-H1A
 1.906145 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C11(H11), C3(H3), C5(H5), C4(H4), C12(H12), C8(H8), C10(H10),
 C9(H9)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              6381
_olex2_submission_special_instructions 'No special instructions were received'