Insight into the conformational selectivity of cobalt(iii) complexes with a tetradentate salen-type Schiff base ligand and their biorelevant catalysis: a combined experimental and theoretical study
Jana, Narayan Ch.; Brandão, Paula; Gomila, Rosa M.; Frontera, Antonio; Panja, Anangamohan; New Journal of Chemistry 48 (2024) 2389–2402; doi:10.1039/D3NJ04609E

data_7062935
_publ_section_title
;
 Insight into the conformational selectivity of cobalt(iii) complexes with
 a tetradentate salen-type Schiff base ligand and their biorelevant
 catalysis: a combined experimental and theoretical study
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2389
_journal_page_last               2402
_journal_paper_doi               10.1039/D3NJ04609E
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety
'3(C32 H36 Co N4 O4), 4.5(H2 O), 3(Cl O4), 1.5(C6 H7 N)'
_chemical_formula_sum            'C105 H127.5 Cl3 Co3 N13.5 O28.5'
_chemical_formula_weight         2317.84
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-12-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2023-12-20 deposited with the CCDC.	2023-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   38.549(4)
_cell_length_b                   38.549(4)
_cell_length_c                   14.2490(14)
_cell_measurement_reflns_used    534
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.99
_cell_volume                     18338(3)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50790
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.431
_diffrn_reflns_theta_min         2.113
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016-2
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             7272
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7473
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0554
_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^)+(0.1272P)^2^+16.7879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.1863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6111
_reflns_number_total             7473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04609e2.cif
_cod_data_source_block           complex-4
_cod_depositor_comments
'Adding full bibliography for 7062933--7062938.cif.'
_cod_original_cell_volume        18338(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C105 H127.50 Cl3 Co3 N13.50 O28.50'
_cod_database_code               7062935
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O10A \\sim O10B \\sim O7A \\sim O7B \\sim O8A \\sim Cl1 \\sim O9A \\sim O8B
\\sim O9B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 1.7A
3. Rigid body (RIGU) restrains
 O7B, O7A, O10B, O10A, O8A, Cl1, O9B, O9A, O8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O7A(0.7) O9A(0.7) O10A(0.7) O8A(0.7) N5(0.5) C35(0.5) C36(0.5)
 H36(0.5) C37(0.5) H37(0.5) C34(0.5) H34(0.5) C33(0.5) H33(0.5) C38(0.5)
 H38A(0.5) H38B(0.5) H38C(0.5) O6(0.5) O7B(0.3) O10B(0.3) O8B(0.3) O9B(0.3)
 H6D(0.5) H6E(0.5)
 Fixed X: H6D(0.71476) H6E(0.7201) H5B(0.728291)
 Fixed Y: H6D(0.42575) H6E(0.39733) H5B(0.472049)
 Fixed Z: H6D(0.75113) H6E(0.79604) H5B(0.5734)
5.a Free rotating group:
 O5(H5A)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B)
5.c Me refined with riding coordinates:
 C38(H38A,H38B,H38C)
5.d Aromatic/amide H refined with riding coordinates:
 C24(H24), C4(H4), C22(H22), C7(H7), C25(H25), C9(H9), C14(H14), C31(H31),
 C27(H27), C21(H21), C30(H30), C12(H12), C17(H17), C28(H28), C36(H36), C37(H37),
  C34(H34), C33(H33)
5.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C),
 C26(H26A,H26B,H26C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              25174
_shelx_hkl_checksum              19194
_shelx_fab_checksum              96587
_olex2_submission_special_instructions 'No special instructions were received'