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_7249282
_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 O2 S, C N S'
_chemical_formula_sum            'C29 H35 Co N7 O2 S2'
_chemical_formula_weight         636.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                84.509(2)
_cell_angle_beta                 85.684(2)
_cell_angle_gamma                69.475(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4553(3)
_cell_length_b                   9.5655(3)
_cell_length_c                   18.0521(5)
_cell_measurement_reflns_used    6450
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      68.1200
_cell_measurement_theta_min      4.9220
_cell_volume                     1520.53(9)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_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    -91.00 -52.00   0.50    3.00    --  -41.99 144.00  20.00   78
  2  \w    -78.00 -21.00   0.50    3.00    --  -41.99 126.00-148.00  114
  3  \w   -100.00 -62.00   0.50    3.00    --  -41.99-144.00 -34.00   76
  4  \w     34.00  69.00   0.50    3.00    --   43.55-126.00 134.00   70
  5  \w     64.00  90.00   0.50    3.00    --   43.55-144.00 -34.00   52
  6  \w     65.00 107.00   0.50    3.00    --   43.55 144.00  20.00   84
  7  \w   -135.00-110.00   0.50   14.00    --  -94.76-144.00 -34.00   50
  8  \w   -105.00 -64.00   0.50   14.00    --  -94.76 126.00-148.00   82
  9  \w   -141.00-116.00   0.50   14.00    --  -94.76-126.00 134.00   50
 10  \w   -105.00 -80.00   0.50   14.00    --  -94.76 144.00  20.00   50
 11  \w     75.00 101.00   0.50   14.00    --   96.32-144.00 -34.00   52
 12  \w     47.00  72.00   0.50   14.00    --   96.32-126.00 134.00   50
 13  \w    103.00 129.00   0.50   14.00    --   96.32 144.00  20.00   52
 14  \w     85.00 151.00   0.50   14.00    --   96.32 126.00-148.00  132
 15  \w   -101.00 -60.00   0.50    3.00    --  -41.99 -65.00  90.00   82
 16  \w   -109.00 -65.00   0.50    3.00    --  -41.99-138.00-120.00   88
 17  \w    -25.00   1.00   0.50    3.00    --  -41.99  11.00-180.00   52
 18  \w      4.00  31.00   0.50    3.00    --  -41.99  11.00-180.00   54
 19  \w    -57.00 -22.00   0.50    3.00    --  -41.99 -65.00  90.00   70
 20  \w    -31.00  -5.00   0.50    3.00    --  -41.99  43.00-120.00   52
 21  \w    -62.00 -14.00   0.50    3.00    --  -41.99  65.00  30.00   96
 22  \w     60.00 107.00   0.50    3.00    --   43.55  77.00-150.00   94
 23  \w    -15.00  11.00   0.50    3.00    --   43.55 -21.00-180.00   52
 24  \w     29.00  56.00   0.50    3.00    --   43.55  77.00-150.00   54
 25  \w     28.00 100.00   0.50    3.00    --   43.55  54.00-180.00  144
 26  \w     68.00  98.00   0.50    3.00    --   43.55 138.00  60.00   60
 27  \w    -22.00   5.00   0.50    3.00    --   43.55 -21.00 120.00   54
 28  \w    -19.00  39.00   0.50    3.00    --   43.55 -43.00 -30.00  116
 29  \w    -10.00  15.00   0.50    3.00    --   43.55 -11.00-120.00   50
 30  \w     68.00  93.00   0.50    3.00    --   43.55 138.00-180.00   50
 31  \w    -68.00 -42.00   0.50   14.00    --  -94.76  59.00-120.00   52
 32  \w    -54.00 -28.00   0.50   14.00    --  -94.76  50.00   0.00   52
 33  \w    -57.00 -32.00   0.50   14.00    --  -94.76  50.00  60.00   50
 34  \w    -53.00 -28.00   0.50   14.00    --  -94.76  50.00 -90.00   50
 35  \w   -156.00 -78.00   0.50   14.00    --  -94.76 -59.00  30.00  156
 36  \w    -56.00 -30.00   0.50   14.00    --  -94.76  50.00 -30.00   52
 37  \w    -68.00 -30.00   0.50   14.00    --  -94.76  59.00 -90.00   76
 38  \w   -114.00 -31.00   0.50   14.00    --  -94.76 144.00   0.00  166
 39  \w   -109.00 -31.00   0.50   14.00    --  -94.76 117.00   0.00  156
 40  \w    -53.00 -28.00   0.50   14.00    --  -94.76  50.00  90.00   50
 41  \w    -65.00 -31.00   0.50   14.00    --  -94.76  59.00  30.00   68
 42  \w     51.00  81.00   0.50   14.00    --   96.32 -68.00 -30.00   60
 43  \w     61.00 110.00   0.50   14.00    --   96.32-117.00 -30.00   98
 44  \w     31.00  57.00   0.50   14.00    --   96.32-117.00 -30.00   52
 45  \w     77.00 148.00   0.50   14.00    --   96.32  50.00-150.00  142
 46  \w     28.00  53.00   0.50   14.00    --   96.32 -59.00 150.00   50
 47  \w     35.00  88.00   0.50   14.00    --   96.32 -77.00 120.00  106
 48  \w     83.00 132.00   0.50   14.00    --   96.32  33.00   0.00   98
 49  \w     31.00  66.00   0.50   14.00    --   96.32 -59.00-120.00   70
 50  \w    108.00 134.00   0.50   14.00    --   96.32  42.00 120.00   52
 51  \w     92.00 125.00   0.50   14.00    --   96.32 -86.00 120.00   66
 52  \w     48.00  81.00   0.50   14.00    --   96.32 -68.00 150.00   66
 53  \w     81.00 106.00   0.50   14.00    --   96.32  42.00 120.00   50
 54  \w     81.00 149.00   0.50   14.00    --   96.32  25.00 -30.00  136
 55  \w     31.00 110.00   0.50   14.00    --   96.32-117.00 150.00  158
 56  \w     83.00 158.00   0.50   14.00    --   96.32  33.00 -90.00  150
 57  \w     85.00 145.00   0.50   14.00    --   96.32  96.00 -90.00  120
 58  \w    134.00 160.00   0.50   14.00    --   96.32  25.00  30.00   52
 59  \w     32.00  57.00   0.50   14.00    --   96.32 -50.00-180.00   50
 60  \w     30.00  55.00   0.50   14.00    --   96.32 -50.00 -30.00   50
 61  \w     28.00  63.00   0.50   14.00    --   96.32 -59.00 -60.00   70
 62  \w     82.00 117.00   0.50   14.00    --   96.32  25.00  30.00   70
 63  \w     30.00  57.00   0.50   14.00    --   96.32 -50.00 120.00   54
 64  \w     44.00 102.00   0.50   14.00    --   96.32 -86.00 -60.00  116
 65  \w     89.00 127.00   0.50   14.00    --   96.32  25.00-180.00   76
;
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14621
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.367
_diffrn_reflns_theta_min         4.927
_exptl_absorpt_coefficient_mu    6.023
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61266
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.465
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         5523
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0624
_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^)+(0.0947P)^2^+1.7622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4906
_reflns_number_total             5523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra02387k2.cif
_cod_data_source_block           04
_cod_original_cell_volume        1520.53(8)
_cod_database_code               7249282
_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. Uiso/Uaniso restraints and constraints
Uanis(S2A) = Uanis(C29A) = Uanis(N7A)
Uanis(N7B) = Uanis(C29B) = Uanis(S2B)
3. Rigid body (RIGU) restrains
 C29A, N7A, S2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29B, N7B, S2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C12, O2A, O2, C12A, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H11C)=Sof(H11D)=Sof(H14C)=Sof(H14D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(O2A)=1-FVAR(1)
 Sof(O2)=Sof(H11A)=Sof(H11B)=Sof(H14A)=Sof(H14B)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(C13)=Sof(H13A)=Sof(H13B)=FVAR(1)
 Sof(C29A)=Sof(N7A)=Sof(S2A)=1-FVAR(2)
 Sof(C29B)=Sof(N7B)=Sof(S2B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C16(H16A,H16B), C8(H8A,H8B), C22(H22A,H22B), C9(H9A,
 H9B), C15(H15A,H15B), C11(H11A,H11B), C11(H11C,H11D), C10(H10A,H10B), C14(H14A,
 H14B), C14(H14C,H14D), C12(H12A,H12B), C13(H13A,H13B), C13A(H13C,H13D),
 C12A(H12C,H12D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2(H2), C21(H21), C18(H18), C27(H27), C19(H19), C20(H20),
 C24(H24), C26(H26), C25(H25)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84093
_shelx_fab_checksum              32308
_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
;