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_7714473
_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         'C17 H29 Co N8, Cl O4'
_chemical_formula_sum            'C17 H29 Cl Co N8 O4'
_chemical_formula_weight         503.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3931(2)
_cell_length_b                   16.2764(2)
_cell_length_c                   17.5144(3)
_cell_measurement_reflns_used    8732
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.8950
_cell_measurement_theta_min      3.9550
_cell_volume                     4388.13(11)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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    -12.00  13.00   0.50    0.48    --  -40.70  39.00 -48.00   50
  2  \w    -28.00  31.00   0.50    0.48    --  -40.70  21.00  30.00  118
  3  \w    -23.00  36.00   0.50    0.48    --  -40.70  11.00  60.00  118
  4  \w    -46.00  20.00   0.50    0.48    --  -40.70  87.00  82.00  132
  5  \w    -60.00 -28.00   0.50    1.93    --  -95.74  59.00-180.00   64
  6  \w    -69.00 -43.00   0.50    1.93    --  -95.74  59.00-150.00   52
  7  \w   -148.00-123.00   0.50    1.93    --  -95.74-109.00  71.00   50
  8  \w   -163.00 -72.00   0.50    1.93    --  -95.74 -59.00  60.00  182
  9  \w    -94.00 -32.00   0.50    0.48    --  -40.70 -39.00 156.00  124
 10  \w    -20.00   9.00   0.50    0.48    --   42.57 -39.00 156.00   58
 11  \w     12.00  43.00   0.50    0.48    --   42.57-109.00  71.00   62
 12  \w     -1.00  24.00   0.50    0.48    --   42.57 -87.00 -35.00   50
 13  \w     47.00  73.00   0.50    1.93    --   97.62-109.00  71.00   52
 14  \w     29.00  69.00   0.50    1.93    --   97.62 -59.00  30.00   80
 15  \w     44.00 115.00   0.50    1.93    --   97.62 -87.00 -35.00  142
 16  \w     30.00  55.00   0.50    1.93    --   97.62 -50.00 -60.00   50
 17  \w     32.00  57.00   0.50    1.93    --   97.62 -50.00 -30.00   50
 18  \w     30.00  57.00   0.50    1.93    --   97.62 -50.00 -90.00   54
 19  \w     29.00  69.00   0.50    1.93    --   97.62 -59.00-120.00   80
 20  \w     48.00  73.00   0.50    0.48    --   42.57  39.00 -48.00   50
 21  \w     98.00 123.00   0.50    1.93    --   97.62  39.00 -48.00   50
 22  \w    123.00 148.00   0.50    1.93    --   97.62  87.00  82.00   50
 23  \w    107.00 141.00   0.50    1.93    --   97.62 109.00 168.00   68
 24  \w     31.00  56.00   0.50    1.93    --   97.62 -50.00 120.00   50
 25  \w     32.00  57.00   0.50    1.93    --   97.62 -50.00  90.00   50
 26  \w     -6.00  20.00   0.50    0.48    --   42.57 -11.00-120.00   52
 27  \w     72.00  98.00   0.50    0.48    --   42.57 138.00-180.00   52
 28  \w    -57.00 -32.00   0.50    0.48    --  -40.70 109.00 168.00   50
 29  \w    -91.00 -66.00   0.50    1.93    --  -95.74 109.00 168.00   50
 30  \w   -151.00 -82.00   0.50    1.93    --  -95.74 -39.00 156.00  138
 31  \w     18.00  43.00   0.50    0.48    --   42.57-109.00  71.00   50
 32  \w    -66.00 -41.00   0.50    0.48    --  -40.70 109.00 168.00   50
 33  \w     18.00  43.00   0.50    0.48    --   42.57-109.00  71.00   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  0.0435
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17155
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         4.691
_exptl_absorpt_coefficient_mu    7.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65462
_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    1.525
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.00076(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0880P)^2^+3.6797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3343
_reflns_number_total             3991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02639f2.cif
_cod_data_source_block           co_03_n3
_cod_database_code               7714473
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.271
_shelx_estimated_absorpt_t_min   0.125
_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:
 N2(H2), N5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C9(H9A,H9B), C6(H6A,H6B), C14(H14A,H14B), C13(H13A,H13B),
 C7(H7A,H7B), C10(H10A,H10B), C15(H15A,H15B), C17(H17A,H17B), C11(H11A,H11B),
 C8(H8A,H8B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C3(H3)
;
_shelx_res_checksum              5214
_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
;