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_7714470
_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 O, Cl O4'
_chemical_formula_sum            'C18 H29 Cl Co N6 O5'
_chemical_formula_weight         503.85
_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                   15.2438(2)
_cell_length_b                   16.37741(19)
_cell_length_c                   17.6591(2)
_cell_measurement_reflns_used    7926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.0300
_cell_measurement_theta_min      4.6800
_cell_volume                     4408.66(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    'SHELXS  (Sheldrick, 2008)'
_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 0.991
_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    -45.00 -19.00   0.50    0.65    --  -40.70  45.00  21.00   52
  2  \w    -69.00 -27.00   0.50    2.60    --  -95.74  59.00 -90.00   84
  3  \w    -57.00 -29.00   0.50    2.60    --  -95.74  50.00-150.00   56
  4  \w    -57.00 -28.00   0.50    2.60    --  -95.74  50.00 -90.00   58
  5  \w    -63.00  -8.00   0.50    0.65    --  -40.70  78.00-152.00  110
  6  \w     60.00  86.00   0.50    0.65    --   42.57  78.00-152.00   52
  7  \w     64.00 108.00   0.50    0.65    --   42.57 138.00-120.00   88
  8  \w     80.00 105.00   0.50    0.65    --   42.57 162.00-117.00   50
  9  \w    118.00 143.00   0.50    2.60    --   97.62  78.00-152.00   50
 10  \w     78.00 154.00   0.50    2.60    --   97.62  45.00  21.00  152
 11  \w     78.00 112.00   0.50    2.60    --   97.62 116.00  92.00   68
 12  \w     43.00  68.00   0.50    0.65    --   42.57  45.00  21.00   50
 13  \w     -6.00  25.00   0.50    0.65    --   42.57 -45.00-129.00   62
 14  \w    -23.00  17.00   0.50    0.65    --   42.57 -21.00-180.00   80
 15  \w     36.00  71.00   0.50    2.60    --   97.62 -68.00 -30.00   70
 16  \w     41.00  67.00   0.50    2.60    --   97.62 -59.00   0.00   52
 17  \w     45.00  70.00   0.50    2.60    --   97.62 -78.00  81.00   50
 18  \w     29.00  67.00   0.50    2.60    --   97.62 -68.00   0.00   76
 19  \w      6.00  40.00   0.50    0.65    --   42.57-116.00   4.00   68
 20  \w    -25.00   0.00   0.50    0.65    --   42.57 -78.00  81.00   50
 21  \w    -91.00 -66.00   0.50    0.65    --  -40.70-138.00  30.00   50
 22  \w   -108.00 -82.00   0.50    0.65    --  -40.70-138.00 -90.00   52
 23  \w    -80.00 -55.00   0.50    0.65    --  -40.70-162.00-144.00   50
 24  \w   -109.00 -83.00   0.50    0.65    --  -40.70-138.00-120.00   52
 25  \w    -64.00 -39.00   0.50    0.65    --  -40.70 -45.00-129.00   50
 26  \w     40.00  66.00   0.50    0.65    --   42.57-162.00-144.00   52
 27  \w    -57.00 -28.00   0.50    2.60    --  -95.74  50.00 150.00   58
 28  \w   -103.00 -63.00   0.50    2.60    --  -95.74 116.00  92.00   80
 29  \w    -89.00 -64.00   0.50    0.65    --  -40.70 162.00-117.00   50
 30  \w    -95.00 -36.00   0.50    2.60    --  -95.74  78.00-152.00  118
 31  \w   -157.00 -78.00   0.50    2.60    --  -95.74 -86.00-180.00  158
 32  \w   -159.00-134.00   0.50    2.60    --  -95.74 -45.00-129.00   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  0.0356
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15682
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.233
_diffrn_reflns_theta_min         4.688
_exptl_absorpt_coefficient_mu    7.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26954
_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    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.415
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0816P)^2^+3.0104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3261
_reflns_number_total             3999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02639f2.cif
_cod_data_source_block           co_04_nco
_cod_original_cell_volume        4408.67(10)
_cod_database_code               7714470
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.376
_shelx_estimated_absorpt_t_min   0.145
_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:
 C6(H6A,H6B), C10(H10A,H10B), C12(H12A,H12B), C7(H7A,H7B), C11(H11A,H11B),
 C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C15(H15A,H15B), C9(H9A,H9B),
 C16(H16A,H16B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2(H2A)
;
_shelx_res_checksum              90556
_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
;