Trigonal prismatic coordination geometry imparted by a macrocyclic ligand: an approach to large axial magnetic anisotropy for Co(II)
Zahradníková, Eva; Sutter, Jean-Pascal; Halaš, Petr; Drahoš, Bohuslav; Dalton Transactions  (2023) –; doi:10.1039/D3DT02639F

data_7714469
_publ_section_title
;
 Trigonal prismatic coordination geometry imparted by a macrocyclic
 ligand: an approach to large axial magnetic anisotropy for Co(II)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02639F
_journal_year                    2023
_chemical_formula_moiety         'C18 H29 Co N6 S, C N S'
_chemical_formula_sum            'C19 H29 Co N7 S2'
_chemical_formula_weight         478.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-04-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-06 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.562(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2598(4)
_cell_length_b                   8.01170(10)
_cell_length_c                   17.7444(4)
_cell_measurement_reflns_used    5731
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.1040
_cell_measurement_theta_min      3.0410
_cell_volume                     2281.99(9)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.976
_diffrn_measured_fraction_theta_max 0.970
_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    -24.00  31.00   0.50    0.60    --   42.57 -41.00  13.00  110
  2  \w     30.00  59.00   0.50    0.60    --   42.57  21.00   0.00   58
  3  \w     64.00 116.00   0.50    0.60    --   42.57  21.00   0.00  104
  4  \w    119.00 166.00   0.50    2.41    --   97.62  42.00 -90.00   94
  5  \w     77.00 111.00   0.50    0.60    --   42.57 138.00 -30.00   68
  6  \w     69.00 101.00   0.50    0.60    --   42.57 138.00 -90.00   64
  7  \w     79.00 113.00   0.50    2.41    --   97.62  42.00 -90.00   68
  8  \w     73.00 102.00   0.50    2.41    --   97.62 -77.00  60.00   58
  9  \w     75.00 100.00   0.50    2.41    --   97.62 -96.00  30.00   50
 10  \w     32.00  57.00   0.50    2.41    --   97.62 -50.00 -60.00   50
 11  \w     30.00  56.00   0.50    2.41    --   97.62 -50.00   0.00   52
 12  \w     22.00  68.00   0.50    2.41    --   97.62 -96.00  30.00   92
 13  \w     -7.00  33.00   0.50    0.60    --   42.57 -43.00-150.00   80
 14  \w    -22.00   3.00   0.50    0.60    --   42.57 -21.00-180.00   50
 15  \w    -70.00 -34.00   0.50    0.60    --  -40.70 -41.00  13.00   72
 16  \w    -57.00 -30.00   0.50    2.41    --  -95.74  50.00 -60.00   54
 17  \w    -57.00 -32.00   0.50    2.41    --  -95.74  50.00 -90.00   50
 18  \w    -57.00 -28.00   0.50    2.41    --  -95.74  50.00-180.00   58
 19  \w    -54.00 -28.00   0.50    2.41    --  -95.74 144.00-180.00   52
 20  \w   -120.00 -62.00   0.50    2.41    --  -95.74 144.00-180.00  116
 21  \w   -138.00 -81.00   0.50    2.41    --  -95.74 -33.00 -60.00  114
 22  \w   -127.00 -83.00   0.50    2.41    --  -95.74 -42.00 -30.00   88
 23  \w   -103.00 -78.00   0.50    0.60    --  -40.70 -41.00  13.00   50
 24  \w     -5.00  20.00   0.50    0.60    --   42.57 -21.00  30.00   50
 25  \w     26.00  52.00   0.50    0.60    --   42.57  41.00 166.00   52
 26  \w     78.00 103.00   0.50    0.60    --   42.57  41.00 166.00   50
 27  \w     87.00 126.00   0.50    2.41    --   97.62  41.00 166.00   78
 28  \w    -45.00  -9.00   0.50    0.60    --  -40.70  41.00 166.00   72
 29  \w    -57.00 -31.00   0.50    2.41    --  -95.74  50.00 120.00   52
 30  \w    -56.00 -30.00   0.50    2.41    --  -95.74  50.00  90.00   52
 31  \w    -57.00 -29.00   0.50    2.41    --  -95.74  50.00 150.00   56
 32  \w    -68.00 -43.00   0.50    2.41    --  -95.74  59.00  90.00   50
 33  \w    -83.00 -46.00   0.50    2.41    --  -95.74  68.00 120.00   74
 34  \w   -104.00 -51.00   0.50    2.41    --  -95.74 144.00 150.00  106
 35  \w   -103.00 -40.00   0.50    2.41    --  -95.74 117.00 150.00  126
 36  \w   -161.00 -80.00   0.50    2.41    --  -95.74 -41.00  13.00  162
 37  \w   -104.00 -79.00   0.50    0.60    --  -40.70-138.00   0.00   50
 38  \w    -89.00 -64.00   0.50    0.60    --  -40.70-138.00 -90.00   50
 39  \w   -108.00 -69.00   0.50    0.60    --  -40.70-138.00-180.00   78
 40  \w   -160.00-135.00   0.50    2.41    --  -95.74 -42.00 -30.00   50
 41  \w    -89.00 -64.00   0.50    0.60    --  -40.70-138.00 150.00   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  0.0563
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9919
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         3.055
_exptl_absorpt_coefficient_mu    7.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32442
_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    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.157
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0958P)^2^+0.1609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3490
_reflns_number_total             4062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02639f2.cif
_cod_data_source_block           co_05_ncs
_cod_original_cell_volume        2281.99(8)
_cod_database_code               7714469
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.375
_shelx_estimated_absorpt_t_min   0.150
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N5(H5), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C11(H11A,H11B), C10(H10A,H10B), C6(H6A,H6B), C7(H7A,H7B),
 C13(H13A,H13B), C12(H12A,H12B), C8(H8A,H8B), C17(H17A,H17B), C15(H15A,H15B),
 C14(H14A,H14B), C9(H9A,H9B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C3(H3)
;
_shelx_res_checksum              43462
_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
;