Synthesis, structural and magnetic properties of cobalt(ii) complexes with pyridine-based macrocyclic ligand containing two pyridine pendant arms
Zahradníková, Eva; Pichon, Céline; Duhayon, Carine; Sutter, Jean-Pascal; Halaš, Petr; Drahoš, Bohuslav; RSC Advances 14 (2024) 28138–28147; doi:10.1039/D4RA02387K

data_7249281
_publ_section_title
;
 Synthesis, structural and magnetic properties of cobalt(ii) complexes
 with pyridine-based macrocyclic ligand containing two pyridine pendant
 arms
;
_journal_issue                   38
_journal_name_full               'RSC Advances'
_journal_page_first              28138
_journal_page_last               28147
_journal_paper_doi               10.1039/D4RA02387K
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C27 H35 Br Co N5 O2, Br'
_chemical_formula_sum            'C27 H35 Br2 Co N5 O2'
_chemical_formula_weight         680.35
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2024-03-28 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.610(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5063(2)
_cell_length_b                   16.1542(6)
_cell_length_c                   19.9926(7)
_cell_measurement_reflns_used    7655
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.6450
_cell_measurement_theta_min      3.5000
_cell_volume                     3055.49(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    -28.00  29.00   0.50    1.62    --  -42.24  21.00  30.00  114
  2  \w    -24.00  21.00   0.50    1.62    --  -42.24  21.00  60.00   90
  3  \w    -35.00  24.00   0.50    1.62    --  -42.24  32.00 -60.00  118
  4  \w    -36.00  26.00   0.50    1.62    --  -42.24  32.00-120.00  124
  5  \w     58.00 103.00   0.50    1.62    --   43.81 146.00-111.00   90
  6  \w     71.00 109.00   0.50    1.62    --   43.81 138.00-180.00   76
  7  \w     87.00 115.00   0.50    6.47    --   95.94 146.00-111.00   56
  8  \w     96.00 162.00   0.50    6.47    --   95.94 117.00 -60.00  132
  9  \w    129.00 164.00   0.50    6.47    --   95.94  68.00  30.00   70
 10  \w    133.00 161.00   0.50    6.47    --   95.94  33.00 -60.00   56
 11  \w     94.00 121.00   0.50    6.47    --   95.94 124.00  82.00   54
 12  \w     85.00 149.00   0.50    6.47    --   95.94  96.00 120.00  128
 13  \w     86.00 163.00   0.50    6.47    --   95.94  33.00 120.00  154
 14  \w     86.00 125.00   0.50    6.47    --   95.94  68.00  30.00   78
 15  \w     83.00 127.00   0.50    6.47    --   95.94  33.00 -60.00   88
 16  \w     74.00 164.00   0.50    6.47    --   95.94  68.00-150.00  180
 17  \w     59.00 155.00   0.50    6.47    --   95.94 145.00 -60.00  192
 18  \w     32.00 110.00   0.50    1.62    --   43.81  54.00  60.00  156
 19  \w     36.00  99.00   0.50    1.62    --   43.81  21.00 -30.00  126
 20  \w     51.00 101.00   0.50    6.47    --   95.94 -77.00  90.00  100
 21  \w     55.00 124.00   0.50    6.47    --   95.94 -86.00   0.00  138
 22  \w     46.00  71.00   0.50    6.47    --   95.94-124.00   3.00   50
 23  \w     29.00  81.00   0.50    6.47    --   95.94-117.00  60.00  104
 24  \w     28.00  68.00   0.50    6.47    --   95.94 -59.00 120.00   80
 25  \w     29.00  55.00   0.50    6.47    --   95.94 -50.00  90.00   52
 26  \w     29.00  54.00   0.50    6.47    --   95.94 -50.00 120.00   50
 27  \w     22.00  54.00   0.50    1.62    --   43.81-124.00   3.00   64
 28  \w     24.00  82.00   0.50    6.47    --   95.94 -96.00   0.00  116
 29  \w     29.00  57.00   0.50    6.47    --   95.94 -50.00 -30.00   56
 30  \w     42.00  67.00   0.50    1.62    --   43.81-146.00-162.00   50
 31  \w    -27.00   6.00   0.50    1.62    --   43.81 -11.00  60.00   66
 32  \w     34.00 100.00   0.50    1.62    --   43.81  43.00 150.00  132
 33  \w    -25.00   0.00   0.50    1.62    --   43.81 -21.00 150.00   50
 34  \w    -45.00   7.00   0.50    1.62    --  -42.24  43.00  90.00  104
 35  \w    -57.00 -31.00   0.50    6.47    --  -94.38  50.00  60.00   52
 36  \w    -57.00 -29.00   0.50    6.47    --  -94.38  50.00  90.00   56
 37  \w    -57.00 -31.00   0.50    6.47    --  -94.38  50.00 150.00   52
 38  \w    -69.00 -29.00   0.50    6.47    --  -94.38  59.00 120.00   80
 39  \w    -74.00 -43.00   0.50    6.47    --  -94.38 124.00  82.00   62
 40  \w    -82.00 -50.00   0.50    6.47    --  -94.38  68.00  90.00   64
 41  \w    -66.00 -38.00   0.50    1.62    --  -42.24 124.00  82.00   56
 42  \w    -61.00 -32.00   0.50    1.62    --  -42.24 138.00  30.00   58
 43  \w    -72.00 -43.00   0.50    6.47    --  -94.38  77.00 -60.00   58
 44  \w    -57.00 -28.00   0.50    6.47    --  -94.38  50.00 -90.00   58
 45  \w    -81.00 -26.00   0.50    6.47    --  -94.38  68.00 -90.00  110
 46  \w    -57.00 -30.00   0.50    6.47    --  -94.38 117.00-120.00   54
 47  \w    -62.00 -33.00   0.50    6.47    --  -94.38 145.00-150.00   58
 48  \w    -97.00 -33.00   0.50    1.62    --  -42.24 138.00-150.00  128
 49  \w    -95.00 -38.00   0.50    6.47    --  -94.38 117.00-180.00  114
 50  \w   -104.00 -53.00   0.50    1.62    --  -42.24 146.00-111.00  102
 51  \w     18.00  83.00   0.50    1.62    --   43.81  77.00-150.00  130
 52  \w     30.00  94.00   0.50    6.47    --   95.94-145.00 150.00  128
 53  \w    -91.00 -62.00   0.50    1.62    --  -42.24-146.00-162.00   58
 54  \w   -103.00 -78.00   0.50    1.62    --  -42.24-138.00-150.00   50
 55  \w   -109.00 -84.00   0.50    1.62    --  -42.24-138.00 -90.00   50
 56  \w   -135.00-110.00   0.50    6.47    --  -94.38-146.00-162.00   50
 57  \w   -121.00 -96.00   0.50    6.47    --  -94.38-124.00   3.00   50
 58  \w    -95.00 -68.00   0.50    1.62    --  -42.24-138.00 120.00   54
 59  \w   -162.00 -80.00   0.50    6.47    --  -94.38 -86.00  60.00  164
 60  \w   -116.00 -54.00   0.50    6.47    --  -94.38  -8.00-150.00  124
 61  \w   -112.00 -46.00   0.50    6.47    --  -94.38 146.00-111.00  132
 62  \w   -120.00 -92.00   0.50    6.47    --  -94.38 139.00 -51.86   56
 63  \w   -127.00 -41.00   0.50    6.47    --  -94.38 145.00-120.00  172
 64  \w   -121.00 -71.00   0.50    6.47    --  -94.38 145.00-150.00  100
 65  \w   -123.00 -77.00   0.50    6.47    --  -94.38 139.00-171.09   92
 66  \w   -127.00 -99.00   0.50    6.47    --  -94.38 145.00   0.00   56
 67  \w   -110.00 -80.00   0.50    6.47    --  -94.38 117.00  90.00   60
 68  \w   -109.00 -56.00   0.50    6.47    --  -94.38 117.00 150.00  106
 69  \w    -69.00 -44.00   0.50    1.62    --  -42.24 138.00 150.00   50
 70  \w   -127.00 -99.00   0.50    6.47    --  -94.38 145.00 120.00   56
 71  \w   -171.00-139.00   0.50    6.47    --  -94.38  -8.00-150.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33103
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.768
_diffrn_reflns_theta_min         3.524
_exptl_absorpt_coefficient_mu    7.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.165
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0895P)^2^+1.8689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4030
_reflns_number_total             5591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra02387k2.cif
_cod_data_source_block           01
_cod_database_code               7249281
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.363
_shelx_estimated_absorpt_t_min   0.159
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C14(H14a,H14b), C16(H16a,H16b), C7(H7a,H7b), C15(H15a,H15b),
 C22(H22a,H22b), C8(H8a,H8b), C9(H9a,H9b), C13(H13a,H13b), C12(H12a,H12b),
 C10(H10a,H10b), C11(H11a,H11b)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C18(H18), C2(H2), C21(H21), C3(H3), C24(H24), C27(H27), C20(H20),
 C25(H25), C19(H19), C26(H26)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70598
_shelx_fab_checksum              6316
_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
;