Probing the redox-conversion of Co(ii)-disulfide to Co(iii)-thiolate complexes: the effect of ligand-field strength
Marvelous, Christian; de Azevedo Santos, Lucas; Siegler, Maxime A.; Fonseca Guerra, Célia; Bouwman, Elisabeth; Dalton Transactions  (2022) –; doi:10.1039/D2DT00356B

data_7710262
_publ_section_title
;
 Probing the redox-conversion of Co(ii)-disulfide to Co(iii)-thiolate
 complexes: the effect of ligand-field strength
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00356B
_journal_year                    2022
_chemical_formula_moiety         'C28 H32 Br4 Co2 N6 S2, C H4 O'
_chemical_formula_sum            'C29 H36 Br4 Co2 N6 O S2'
_chemical_formula_weight         986.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-04 deposited with the CCDC.	2022-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.345(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7651(7)
_cell_length_b                   11.9665(5)
_cell_length_c                   19.6343(8)
_cell_measurement_reflns_used    5527
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.8480
_cell_measurement_theta_min      2.7250
_cell_volume                     3604.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28658
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.008
_exptl_absorpt_coefficient_mu    5.504
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue-purple
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_description       'small plate'
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.936
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6355
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0537P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4720
_reflns_number_total             6355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00356b2.cif
_cod_data_source_block           1Br_revised
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710262
_shelx_shelxl_version_number     2018/3
_oxdiff_exptl_absorpt_empirical_full_min 0.795
_oxdiff_exptl_absorpt_empirical_full_max 1.386
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              25076
_shelx_hkl_checksum              70351