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_7249284
_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         'C28 H35 Co N6 O3, Cl O4'
_chemical_formula_sum            'C28 H35 Cl Co N6 O7'
_chemical_formula_weight         662.00
_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                 93.777(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1831(3)
_cell_length_b                   15.8178(4)
_cell_length_c                   19.9190(6)
_cell_measurement_reflns_used    6958
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.3410
_cell_measurement_theta_min      3.5520
_cell_volume                     3201.47(16)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.982
_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    -75.00   3.00   0.50    1.00    --  -42.75 105.00-101.00  156
  2  \w     -3.00  78.00   0.50    1.00    --   44.32-105.00 157.00  162
  3  \w   -107.00 -78.00   0.50    4.40    --  -95.95 105.00-101.00   58
  4  \w     30.00  98.00   0.50    4.40    --   97.51-105.00 157.00  136
  5  \w     83.00 125.00   0.50    4.40    --   97.51 105.00-101.00   84
  6  \w    -34.00  23.00   0.50    1.00    --  -42.75  32.00  30.00  114
  7  \w     76.00 113.00   0.50    1.00    --   44.32  77.00-120.00   74
  8  \w    -25.00  28.00   0.50    1.00    --   44.32 -21.00 120.00  106
  9  \w     66.00 111.00   0.50    1.00    --   44.32 138.00-180.00   90
 10  \w    -21.00  19.00   0.50    1.00    --   44.32 -21.00  60.00   80
 11  \w     20.00  75.00   0.50    1.00    --   44.32  77.00-120.00  110
 12  \w    -68.00 -29.00   0.50    4.40    --  -95.95  59.00-150.00   78
 13  \w    -78.00 -29.00   0.50    4.40    --  -95.95  68.00 -90.00   98
 14  \w   -161.00-115.00   0.50    4.40    --  -95.95 -42.00   0.00   92
 15  \w    -77.00 -29.00   0.50    4.40    --  -95.95  68.00 150.00   96
 16  \w   -108.00 -82.00   0.50    4.40    --  -95.95 -42.00   0.00   52
 17  \w   -106.00 -30.00   0.50    4.40    --  -95.95  77.00  90.00  152
 18  \w    -68.00 -30.00   0.50    4.40    --  -95.95  59.00-120.00   76
 19  \w     30.00 105.00   0.50    4.40    --   97.51 -77.00 150.00  150
 20  \w     84.00 163.00   0.50    4.40    --   97.51  42.00-150.00  158
 21  \w     85.00 167.00   0.50    4.40    --   97.51  17.00 120.00  164
 22  \w     88.00 163.00   0.50    4.40    --   97.51  33.00-180.00  150
;
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15118
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.694
_diffrn_reflns_theta_min         3.571
_exptl_absorpt_coefficient_mu    5.416
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30345
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         5926
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0929P)^2^+1.6055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4687
_reflns_number_total             5926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra02387k2.cif
_cod_data_source_block           03
_cod_original_cell_volume        3201.46(17)
_cod_database_code               7249284
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.565
_shelx_estimated_absorpt_t_min   0.207
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid body (RIGU) restrains
 O3, O3A, O6A, O6, O5A, O5, O4A, O4, Cl1, Cl1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(O3A)=Sof(Cl1A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=1-FVAR(1)
 Sof(Cl1)=Sof(O6)=Sof(O5)=Sof(O3)=Sof(O4)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B), C16(H16A,H16B), C15(H15A,H15B), C7(H7A,H7B),
 C22(H22A,H22B), C8(H8A,H8B), C13(H13A,H13B), C12(H12A,H12B), C9(H9A,H9B),
 C11(H11A,H11B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C3(H3), C21(H21), C27(H27), C18(H18), C19(H19), C26(H26),
 C20(H20), C24(H24), C25(H25)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              66094
_shelx_fab_checksum              21629
_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
;