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_7714468
_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 Cl Co N5, Cl, C H4 O'
_chemical_formula_sum            'C18 H33 Cl2 Co N5 O'
_chemical_formula_weight         465.32
_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                   10.7580(2)
_cell_length_b                   13.7934(3)
_cell_length_c                   31.8783(6)
_cell_measurement_reflns_used    8649
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.0740
_cell_measurement_theta_min      2.7590
_cell_volume                     4730.40(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.994
_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    -14.00  30.00   0.50    1.57    --  -40.70  26.00 -21.00   88
  2  \w    -49.00 -24.00   0.50    1.57    --  -40.70  98.00 144.00   50
  3  \w    -69.00 -27.00   0.50    6.27    --  -95.74  59.00  90.00   84
  4  \w    -55.00 -29.00   0.50    6.27    --  -95.74  50.00  30.00   52
  5  \w    -97.00 -26.00   0.50    1.57    --  -40.70 -26.00 174.00  142
  6  \w   -108.00 -83.00   0.50    1.57    --  -40.70-146.00 153.00   50
  7  \w    -91.00 -66.00   0.50    1.57    --  -40.70-138.00  90.00   50
  8  \w   -138.00 -90.00   0.50    6.27    --  -95.74-125.00 -40.00   96
  9  \w   -157.00 -74.00   0.50    6.27    --  -95.74 -68.00 120.00  166
 10  \w   -147.00-122.00   0.50    6.27    --  -95.74 -26.00 174.00   50
 11  \w   -107.00 -53.00   0.50    6.27    --  -95.74  98.00 144.00  108
 12  \w   -101.00 -29.00   0.50    1.57    --  -40.70 138.00 -30.00  144
 13  \w    -82.00 -56.00   0.50    1.57    --  -40.70 146.00-155.00   52
 14  \w   -101.00 -76.00   0.50    6.27    --  -95.74 146.00-155.00   50
 15  \w    -57.00 -29.00   0.50    6.27    --  -95.74  50.00-120.00   56
 16  \w     59.00  84.00   0.50    1.57    --   42.57-146.00 153.00   50
 17  \w     53.00  78.00   0.50    6.27    --   97.62-146.00 153.00   50
 18  \w     33.00  83.00   0.50    6.27    --   97.62 -68.00  30.00  100
 19  \w     29.00  56.00   0.50    6.27    --   97.62 -59.00 -60.00   54
 20  \w     31.00  57.00   0.50    6.27    --   97.62 -59.00 -90.00   52
 21  \w     30.00  55.00   0.50    6.27    --   97.62 -50.00-150.00   50
 22  \w     29.00  62.00   0.50    6.27    --   97.62 -59.00-180.00   66
 23  \w     25.00  51.00   0.50    1.57    --   42.57  26.00 -21.00   52
 24  \w     80.00 155.00   0.50    6.27    --   97.62  26.00 -21.00  150
 25  \w    112.00 151.00   0.50    6.27    --   97.62  98.00 144.00   78
 26  \w     75.00 100.00   0.50    1.57    --   42.57 138.00   0.00   50
 27  \w     63.00  88.00   0.50    1.57    --   42.57 146.00-155.00   50
 28  \w     69.00 103.00   0.50    1.57    --   42.57 138.00-180.00   68
 29  \w     -9.00  17.00   0.50    1.57    --   42.57 -32.00 120.00   52
 30  \w      7.00  32.00   0.50    1.57    --   42.57 -98.00  36.00   50
 31  \w     30.00  55.00   0.50    6.27    --   97.62 -50.00 150.00   50
 32  \w    -22.00   3.00   0.50    1.57    --   42.57 -26.00 174.00   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  0.0533
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            17798
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.104
_diffrn_reflns_theta_min         2.772
_exptl_absorpt_coefficient_mu    7.896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20660
_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 orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.582
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.278
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0541
_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^)+(0.1116P)^2^+0.4990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3456
_reflns_number_total             4291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02639f2.cif
_cod_data_source_block           co_01_cl
_cod_original_cell_volume        4730.38(16)
_cod_database_code               7714468
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.218
_shelx_estimated_absorpt_t_min   0.091
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 N5(H5), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C6(H6A,H6B), C16(H16A,H16B), C11(H11A,H11B), C13(H13A,H13B),
 C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B),
 C8(H8A,H8B), C15(H15A,H15B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C3(H3)
2.d Tetrahedral OH refined with riding coordinates:
 O1(H1)
2.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99183
_shelx_fab_checksum              14051
_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
;