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_7062938
_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         '2(C30 H31.5 Co N4 O6), 2(H2 O), Cl O4'
_chemical_formula_sum            'C60 H67 Cl Co2 N8 O18'
_chemical_formula_weight         1341.52
_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     dual
_audit_creation_date             2023-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-12 deposited with the CCDC.	2023-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.537(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3579(5)
_cell_length_b                   20.4126(3)
_cell_length_c                   14.2746(3)
_cell_measurement_reflns_used    30755
_cell_measurement_temperature    297.5(6)
_cell_measurement_theta_max      77.1500
_cell_measurement_theta_min      3.8510
_cell_volume                     7118.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      297.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -107.00 -35.00   0.50    4.95    --  -38.50 -30.00 -11.00  144
  2  \w    -42.00  30.00   0.50    4.95    --  -38.50  30.00 148.00  144
  3  \w    -19.00  53.00   0.50    4.95    --   49.31 -30.00 -11.00  144
  4  \w     46.00 118.00   0.50    4.95    --   49.31  30.00 148.00  144
  5  \w     39.00 111.00   0.50   21.45    --  107.46 -30.00 -11.00  144
  6  \w    104.00 176.00   0.50   21.45    --  107.46  30.00 148.00  144
  7  \w    -44.00  31.00   0.50    4.95    --  -38.50  19.00 -60.00  150
  8  \w     46.00 116.00   0.50    4.95    --   49.31  37.00-180.00  140
  9  \w    -13.00  61.00   0.50    4.95    --   49.31 -57.00-120.00  148
 10  \w    103.00 172.00   0.50   21.45    --  107.46  77.00   0.00  138
 11  \w     43.00 113.00   0.50   21.45    --  107.46-125.00 150.00  140
 12  \w    103.00 172.00   0.50   21.45    --  107.46  77.00  90.00  138
 13  \w     97.00 172.00   0.50   21.45    --  107.46 125.00  30.00  150
 14  \w     45.00 121.00   0.50   21.45    --  107.46 -61.00 150.00  152
 15  \w    104.00 176.00   0.50   21.45    --  107.46  30.00  30.00  144
 16  \w    103.00 172.00   0.50   21.45    --  107.46  77.00 150.00  138
 17  \w     39.00 107.00   0.50   21.45    --  107.46 -94.00 -90.00  136
 18  \w     45.00 121.00   0.50   21.45    --  107.46 -61.00  90.00  152
 19  \w     43.00 112.00   0.50   21.45    --  107.46 -45.00 150.00  138
 20  \w     38.00 112.00   0.50    4.95    --   49.31  57.00-120.00  148
 21  \w     38.00 112.00   0.50    4.95    --   49.31  57.00   0.00  148
 22  \w     38.00  88.00   0.50    4.95    --   49.31  57.00  60.00  100
 23  \w     38.00 112.00   0.50    4.95    --   49.31  57.00 -60.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            71337
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.687
_diffrn_reflns_theta_min         3.618
_exptl_absorpt_coefficient_mu    4.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.52a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         14837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0756
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1445P)^2^+6.3473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2167
_refine_ls_wR_factor_ref         0.2417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10808
_reflns_number_total             14837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04609e2.cif
_cod_data_source_block           complex-5
_cod_depositor_comments
'Adding full bibliography for 7062933--7062938.cif.'
_cod_database_code               7062938
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.658
_shelx_estimated_absorpt_t_min   0.462
_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) groups
2.a Free rotating group:
 O7(H7A,H7B), O14(H14A,H14B)
2.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C10(H10A,H10B), C41(H41A,H41B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C21(H21), C50(H50), C26(H26), C54(H54), C25(H25), C27(H27),
 C12(H12), C7(H7), C59(H59), C55(H55), C24(H24), C22(H22), C52(H52), C51(H51),
 C60(H60), C9(H9), C57(H57), C4(H4), C30(H30), C47(H47), C56(H56), C39(H39),
 C29(H29), C20(H20), C34(H34), C17(H17), C37(H37)
2.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C46(H46A,H46B,H46C), C6(H6A,H6B,H6C), C49(H49A,H49B,H49C),
 C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C19(H19A,H19B,H19C), C36(H36A,H36B,
 H36C)
2.e Idealised tetrahedral OH refined as rotating group:
 O6'(H6'), O6(H6)
;
_shelx_res_checksum              31477
_shelx_hkl_checksum              38145
_shelx_fab_checksum              53607
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;