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_7249285
_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 N8 O2, Cl O4'
_chemical_formula_sum            'C27 H35 Cl Co N8 O6'
_chemical_formula_weight         662.01
_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_date             2024-03-28
_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                 95.297(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2781(4)
_cell_length_b                   15.7954(4)
_cell_length_c                   19.6987(5)
_cell_measurement_reflns_used    6415
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      68.6650
_cell_measurement_theta_min      3.5920
_cell_volume                     3184.36(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(13)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.977
_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    -90.00 -56.00   0.50    5.00    --  -43.75 149.00-101.00   68
  2  \w   -107.00 -59.00   0.50    5.00    --  -43.75-149.00-147.00   96
  3  \w     11.00  89.00   0.50    5.00    --   45.32-122.00  14.00  156
  4  \w     64.00  90.00   0.50    5.00    --   45.32 149.00-101.00   52
  5  \w     52.00  77.00   0.50    5.00    --   45.32-149.00-147.00   50
  6  \w   -111.00 -86.00   0.50   13.00    --  -95.95-149.00-147.00   50
  7  \w   -103.00 -78.00   0.50   13.00    --  -95.95 149.00-101.00   50
  8  \w   -143.00-118.00   0.50   13.00    --  -95.95-122.00  14.00   50
  9  \w     71.00 104.00   0.50   13.00    --   97.51-122.00  14.00   66
 10  \w    100.00 162.00   0.50   13.00    --   97.51 122.00  95.00  124
 11  \w    -74.00 -30.00   0.50    5.00    --  -43.75 -43.00  30.00   88
 12  \w   -111.00 -25.00   0.50    5.00    --  -43.75 -77.00   0.00  172
 13  \w    -25.00  26.00   0.50    5.00    --  -43.75  11.00 -30.00  102
 14  \w   -107.00 -80.00   0.50    5.00    --  -43.75 -43.00  30.00   54
 15  \w    -25.00  30.00   0.50    5.00    --  -43.75  11.00  90.00  110
 16  \w    -24.00  26.00   0.50    5.00    --   45.32 -21.00-120.00  100
 17  \w    -69.00 -29.00   0.50   13.00    --  -95.95  59.00 -90.00   80
 18  \w   -162.00 -87.00   0.50   13.00    --  -95.95 -42.00  90.00  150
 19  \w    -55.00 -29.00   0.50   13.00    --  -95.95  50.00 150.00   52
 20  \w    -81.00 -32.00   0.50   13.00    --  -95.95  68.00 -60.00   98
 21  \w    -54.00 -29.00   0.50   13.00    --  -95.95  50.00 -60.00   50
 22  \w   -162.00 -84.00   0.50   13.00    --  -95.95 -42.00-150.00  156
 23  \w    -57.00 -29.00   0.50   13.00    --  -95.95  50.00-120.00   56
 24  \w     84.00 169.00   0.50   13.00    --   97.51  17.00 150.00  170
 25  \w     31.00  68.00   0.50   13.00    --   97.51 -59.00 150.00   74
 26  \w     41.00  82.00   0.50   13.00    --   97.51 -68.00   0.00   82
 27  \w     32.00 126.00   0.50   13.00    --   97.51 -86.00   0.00  188
 28  \w   -113.00 -64.00   0.50   13.00    --  -95.95 125.00  -1.00   98
 29  \w    109.00 153.00   0.50   13.00    --   97.51  33.00-150.00   88
;
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16491
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.917
_diffrn_reflns_theta_min         3.593
_exptl_absorpt_coefficient_mu    5.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       plate
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         5884
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0639
_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^)+(0.1230P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.1869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4143
_reflns_number_total             5884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra02387k2.cif
_cod_data_source_block           05
_cod_database_code               7249285
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Rigid body (RIGU) restrains
 O4, O4A, O3A, O6, Cl1A, Cl1, O5A, O3, O5, O6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C12A, O2A, O2, C11A, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(Cl1A)=Sof(O4A)=Sof(O6A)=Sof(O5A)=Sof(O3A)=1-FVAR(1)
 Sof(Cl1)=Sof(O3)=Sof(O5)=Sof(O6)=Sof(O4)=FVAR(1)
 Sof(H13C)=Sof(H13D)=Sof(H10C)=Sof(H10D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=
 Sof(O2A)=Sof(C11A)=Sof(H11C)=Sof(H11D)=1-FVAR(2)
 Sof(O2)=Sof(H13A)=Sof(H13B)=Sof(H10A)=Sof(H10B)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C15(H15A,H15B), C6(H6A,H6B), C14(H14A,H14B), C7(H7A,H7B),
 C16(H16A,H16B), C8(H8A,H8B), C13(H13A,H13B), C13(H13C,H13D), C9(H9A,H9B),
 C10(H10A,H10B), C10(H10C,H10D), C12(H12A,H12B), C11(H11A,H11B), C12A(H12C,
 H12D), C11A(H11C,H11D)
4.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C2(H2), C24(H24), C4(H4), C21(H21), C25(H25), C3(H3), C26(H26),
 C18(H18), C20(H20), C19(H19)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48200
_shelx_fab_checksum              65598
_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
;