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_7714474
_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 Se, C N Se'
_chemical_formula_sum            'C19 H29 Co N7 Se2'
_chemical_formula_weight         572.34
_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                 111.654(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3749(2)
_cell_length_b                   8.20480(10)
_cell_length_c                   17.9050(2)
_cell_measurement_reflns_used    8656
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.1750
_cell_measurement_theta_min      3.0220
_cell_volume                     2372.36(6)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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      6.00  44.00   0.50    0.50    --   42.57 -43.00 -90.00   76
  2  \w     80.00 155.00   0.50    2.00    --   97.62  50.00  60.00  150
  3  \w    140.00 167.00   0.50    2.00    --   97.62  33.00  90.00   54
  4  \w     93.00 166.00   0.50    2.00    --   97.62  33.00 120.00  146
  5  \w    -29.00  17.00   0.50    0.50    --   42.57 -21.00 150.00   92
  6  \w    -33.00  12.00   0.50    0.50    --   42.57 -11.00  90.00   90
  7  \w     -4.00  25.00   0.50    0.50    --   42.57 -11.00-150.00   58
  8  \w    -16.00  21.00   0.50    0.50    --   42.57 -11.00-180.00   74
  9  \w     13.00  75.00   0.50    0.50    --   42.57 -89.00-180.00  124
 10  \w     46.00 101.00   0.50    0.50    --   42.57-138.00  25.00  110
 11  \w     37.00  78.00   0.50    0.50    --   42.57-131.00-159.00   82
 12  \w    -29.00   4.00   0.50    0.50    --   42.57 -89.00-180.00   66
 13  \w     52.00  77.00   0.50    2.00    --   97.62-138.00  25.00   50
 14  \w     31.00  57.00   0.50    2.00    --   97.62 -50.00 150.00   52
 15  \w     29.00 109.00   0.50    2.00    --   97.62-117.00  30.00  160
 16  \w     30.00  57.00   0.50    2.00    --   97.62 -50.00  60.00   54
 17  \w     35.00  69.00   0.50    2.00    --   97.62 -59.00   0.00   68
 18  \w     36.00  74.00   0.50    2.00    --   97.62-131.00-159.00   76
 19  \w     57.00  83.00   0.50    2.00    --   97.62 -77.00-180.00   52
 20  \w     31.00  57.00   0.50    2.00    --   97.62 -50.00-150.00   52
 21  \w     64.00 111.00   0.50    0.50    --   42.57 138.00  87.00   94
 22  \w     91.00 116.00   0.50    2.00    --   97.62 138.00  87.00   50
 23  \w     13.00  41.00   0.50    0.50    --   42.57  91.00 147.27   56
 24  \w   -101.00 -19.00   0.50    0.50    --  -40.70 138.00  87.00  164
 25  \w   -122.00 -28.00   0.50    2.00    --  -95.74 138.00  87.00  188
 26  \w   -110.00 -27.00   0.50    2.00    --  -95.74 117.00  90.00  166
 27  \w    -96.00 -15.00   0.50    0.50    --  -40.70 131.00 -87.00  162
 28  \w   -114.00 -34.00   0.50    2.00    --  -95.74 131.00 -87.00  160
 29  \w   -105.00 -57.00   0.50    2.00    --  -95.74  77.00 -60.00   96
 30  \w    -81.00 -40.00   0.50    2.00    --  -95.74  68.00-120.00   82
 31  \w    -28.00  23.00   0.50    0.50    --  -40.70  21.00-150.00  102
 32  \w      1.00  27.00   0.50    0.50    --  -40.70  43.00  90.00   52
 33  \w    -49.00  -3.00   0.50    0.50    --  -40.70  43.00  90.00   92
 34  \w   -160.00 -75.00   0.50    2.00    --  -95.74 -78.00 -68.07  170
 35  \w    -42.00  -9.00   0.50    0.50    --  -40.70 -90.00  47.86   66
 36  \w    -91.00 -65.00   0.50    2.00    --  -95.74-138.00  25.00   52
 37  \w   -107.00 -67.00   0.50    0.50    --  -40.70-138.00-180.00   80
 38  \w   -154.00-110.00   0.50    2.00    --  -95.74 -96.00 -30.00   88
 39  \w    -43.00 -11.00   0.50    0.50    --  -40.70 -84.00 179.90   64
;
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13917
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.066
_diffrn_reflns_theta_min         3.029
_exptl_absorpt_coefficient_mu    9.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18159
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       plate
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0606P)^2^+1.9934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3873
_reflns_number_total             4287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02639f2.cif
_cod_data_source_block           co_06_ncse
_cod_database_code               7714474
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.530
_shelx_estimated_absorpt_t_min   0.124
_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:
 C11(H11A,H11B), C16(H16A,H16B), C10(H10A,H10B), C17(H17A,H17B), C13(H13A,
 H13B), C6(H6A,H6B), C12(H12A,H12B), C7(H7A,H7B), C9(H9A,H9B), C14(H14A,H14B),
 C8(H8A,H8B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C3(H3)
;
_shelx_res_checksum              58976
_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
;