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_7062936
_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         'C30 H34 Co N6 O4, Cl O4, 0.65(H2 O), 0.35(O1)'
_chemical_formula_sum            'C30 H35.3 Cl Co N6 O9'
_chemical_formula_weight         718.32
_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                 107.4360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.06470(10)
_cell_length_b                   16.8600(2)
_cell_length_c                   17.5562(2)
_cell_measurement_reflns_used    19625
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.0300
_cell_measurement_theta_min      3.7140
_cell_volume                     3124.64(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_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   -106.00 -21.00   0.50    0.24    --  -38.50 153.00-129.00  170
  2  \w    -85.00  -3.00   0.50    0.24    --  -38.50 121.00  70.00  164
  3  \w     42.00 118.00   0.50    0.24    --   49.56-153.00-171.00  152
  4  \w     80.00 164.00   0.50    1.50    --  107.46 153.00-129.00  168
  5  \w     44.00 110.00   0.50    1.50    --  107.46-121.00 -12.00  132
  6  \w     44.00 132.00   0.50    1.50    --  107.46-153.00-171.00  176
  7  \w     99.00 171.00   0.50    1.50    --  107.46 121.00  70.00  144
  8  \w   -101.00 -27.00   0.50    0.24    --  -38.50 -57.00-120.00  148
  9  \w    -44.00  31.00   0.50    0.24    --  -38.50  19.00-150.00  150
 10  \w     24.00  96.00   0.50    0.24    --   49.56-121.00 -12.00  144
 11  \w     46.00 116.00   0.50    0.24    --   49.56  37.00-150.00  140
 12  \w     45.00 113.00   0.50    1.50    --  107.46-125.00-150.00  136
 13  \w    103.00 172.00   0.50    1.50    --  107.46  77.00-180.00  138
 14  \w     39.00 116.00   0.50    1.50    --  107.46 -15.00 -30.00  154
 15  \w     97.00 170.00   0.50    1.50    --  107.46 125.00 -90.00  146
 16  \w     39.00 107.00   0.50    1.50    --  107.46 -94.00   0.00  136
 17  \w     39.00 116.00   0.50    1.50    --  107.46 -15.00 -90.00  154
 18  \w     39.00 111.00   0.50    1.50    --  107.46 -30.00-180.00  144
 19  \w     45.00 113.00   0.50    1.50    --  107.46-125.00  90.00  136
 20  \w     43.00 112.00   0.50    1.50    --  107.46 -45.00 -60.00  138
 21  \w     43.00 112.00   0.50    1.50    --  107.46 -45.00 150.00  138
 22  \w     38.00 113.00   0.50    0.24    --   49.56  57.00  60.00  150
;
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32569
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.200
_diffrn_reflns_theta_min         3.720
_exptl_absorpt_coefficient_mu    5.650
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             1493
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0760P)^2^+2.7928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1319
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6172
_reflns_number_total             6546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj04609e2.cif
_cod_data_source_block           complex-6
_cod_depositor_comments
'Adding full bibliography for 7062933--7062938.cif.'
_cod_original_formula_sum        'C30 H35.30 Cl Co N6 O9'
_cod_database_code               7062936
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.398
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O6(0.65) H6F(0.65) H6G(0.65) O5(0.35)
3.a Free rotating group:
 O6(H6F,H6G)
3.b Rotating group:
 N5(H5A,H5B), N6(H6A,H6B)
3.c Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B)
3.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C24(H24), C20(H20), C25(H25), C22(H22), C21(H21), C26(H26), C27(H27),
 C17(H17), C7(H7), C29(H29), C30(H30), C12(H12), C4(H4)
3.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C6(H6C,H6D,H6E), C19(H19A,H19B,H19C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              35979
_shelx_hkl_checksum              3457
_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
;