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_7249283
_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 Co I N5 O2, 0.513(Cl O4), 0.487(I)'
_chemical_formula_sum            'C27 H35 Cl0.51 Co I1.49 N5 O4.05'
_chemical_formula_weight         760.30
_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
_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                 92.489(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8084(2)
_cell_length_b                   16.5786(3)
_cell_length_c                   20.3177(3)
_cell_measurement_reflns_used    8395
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.1630
_cell_measurement_theta_min      3.4240
_cell_volume                     3300.73(10)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.983
_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     -2.00  24.00   0.50    0.44    --   42.82 -34.00 -39.00   52
  2  \w    -18.00  24.00   0.50    0.44    --   42.82 -11.00 -30.00   84
  3  \w    -25.00  37.00   0.50    0.44    --   42.82 -32.00-120.00  124
  4  \w     31.00  63.00   0.50    1.75    --   97.62 -77.00-180.00   64
  5  \w     67.00 103.00   0.50    1.75    --   97.62 -77.00-180.00   72
  6  \w     47.00  73.00   0.50    1.75    --   97.62 -68.00-180.00   52
  7  \w     36.00  69.00   0.50    1.75    --   97.62 -59.00 -60.00   66
  8  \w     79.00 166.00   0.50    1.75    --   97.62  42.00-150.00  174
  9  \w     78.00 110.00   0.50    0.44    --   42.82  65.00-120.00   64
 10  \w     64.00 110.00   0.50    0.44    --   42.82 138.00 -30.00   92
 11  \w     64.00  99.00   0.50    0.44    --   42.82 138.00   0.00   70
 12  \w     27.00  59.00   0.50    0.44    --   42.82  34.00 117.00   64
 13  \w     66.00 103.00   0.50    0.44    --   42.82  34.00 117.00   74
 14  \w     82.00 149.00   0.50    1.75    --   97.62  34.00 117.00  134
 15  \w     99.00 131.00   0.50    1.75    --   97.62  33.00  90.00   64
 16  \w     64.00 111.00   0.50    0.44    --   42.82 138.00 150.00   94
 17  \w     -2.00  29.00   0.50    0.44    --  -40.95  65.00 -30.00   62
 18  \w    -30.00  -4.00   0.50    0.44    --  -40.95 104.00 -60.00   52
 19  \w    -54.00 -28.00   0.50    1.75    --  -95.74  50.00  60.00   52
 20  \w    -57.00 -28.00   0.50    1.75    --  -95.74  50.00   0.00   58
 21  \w    -67.00 -32.00   0.50    1.75    --  -95.74  59.00  30.00   70
 22  \w    -57.00 -29.00   0.50    1.75    --  -95.74  50.00  90.00   56
 23  \w    -67.00 -38.00   0.50    1.75    --  -95.74  59.00 150.00   58
 24  \w    -71.00 -45.00   0.50    1.75    --  -95.74  68.00  60.00   52
 25  \w    -82.00 -44.00   0.50    1.75    --  -95.74  68.00 120.00   76
 26  \w      2.00  27.00   0.50    0.44    --  -40.95  34.00 117.00   50
 27  \w    -59.00 -26.00   0.50    0.44    --  -40.95  65.00 -30.00   66
 28  \w    -57.00 -30.00   0.50    1.75    --  -95.74  50.00-120.00   54
 29  \w    -68.00 -39.00   0.50    1.75    --  -95.74  59.00-150.00   58
 30  \w    -79.00 -54.00   0.50    0.44    --  -40.95 104.00 -60.00   50
 31  \w     22.00  47.00   0.50    0.44    --   42.82  65.00-120.00   50
 32  \w     55.00  80.00   0.50    0.44    --   42.82-104.00 120.00   50
 33  \w      4.00  29.00   0.50    0.44    --   42.82-104.00 120.00   50
 34  \w    -66.00 -37.00   0.50    0.44    --  -40.95 -34.00 -39.00   58
 35  \w   -106.00 -21.00   0.50    1.75    --  -95.74  96.00 120.00  170
 36  \w   -110.00 -29.00   0.50    1.75    --  -95.74 117.00 120.00  162
 37  \w   -121.00 -81.00   0.50    1.75    --  -95.74 -34.00 -39.00   80
 38  \w   -140.00 -77.00   0.50    1.75    --  -95.74 -25.00 -90.00  126
 39  \w   -158.00-114.00   0.50    1.75    --  -95.74 -33.00-150.00   88
 40  \w    -24.00   2.00   0.50    0.44    --   42.57 -34.00 -39.00   52
 41  \w    -54.00 -28.00   0.50    1.75    --  -95.74  50.00 -90.00   52
 42  \w     30.00  55.00   0.50    1.75    --   97.62 -50.00 150.00   50
;
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17924
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.559
_diffrn_reflns_theta_min         3.442
_exptl_absorpt_coefficient_mu    15.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32579
_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    1.530
_exptl_crystal_description       prism
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0719P)^2^+3.6801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5013
_reflns_number_total             5979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra02387k2.cif
_cod_data_source_block           02
_cod_database_code               7249283
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.243
_shelx_estimated_absorpt_t_min   0.100
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Sof(I2)=1-FVAR(1)
 Sof(Cl2)=Sof(O5)=Sof(O3)=Sof(O4)=Sof(O6)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C22(H22A,H22B), C16(H16A,H16B), C6(H6A,H6B), C7(H7A,H7B),
 C14(H14A,H14B), C8(H8A,H8B), C12(H12A,H12B), C13(H13A,H13B), C9(H9A,H9B),
 C11(H11A,H11B), C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C18(H18), C27(H27), C24(H24), C2(H2), C21(H21), C19(H19), C3(H3),
 C26(H26), C20(H20), C25(H25)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 68 electrons were 
found in a volume of 514\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3OH] per Asymmetric Unit 
which account for 72 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58735
_shelx_fab_checksum              11103
_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
;