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_7714472
_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 Br Co N5, 0.5(C H4 O), Br'
_chemical_formula_sum            'C17.5 H31 Br2 Co N5 O0.5'
_chemical_formula_weight         538.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 90.7236(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.5309(4)
_cell_length_b                   10.45941(15)
_cell_length_c                   14.18701(16)
_cell_measurement_reflns_used    11374
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.9700
_cell_measurement_theta_min      3.1120
_cell_volume                     4233.30(10)
_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 0.991
_diffrn_measured_fraction_theta_max 0.983
_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    -26.00  32.00   0.50    1.08    --  -40.95  21.00 -30.00  116
  2  \w    -27.00  32.00   0.50    1.08    --  -40.95  21.00 -90.00  118
  3  \w    -24.00  35.00   0.50    1.08    --  -40.95  11.00  60.00  118
  4  \w     24.00  82.00   0.50    1.08    --   42.82-104.00 150.00  116
  5  \w     42.00  68.00   0.50    4.31    --   97.62 -59.00  30.00   52
  6  \w     49.00  82.00   0.50    4.31    --   97.62 -68.00  90.00   66
  7  \w     31.00 111.00   0.50    4.31    --   97.62-121.00  28.00  160
  8  \w     57.00  82.00   0.50    1.08    --   42.82-153.00-130.00   50
  9  \w    107.00 132.00   0.50    4.31    --   97.62-153.00-130.00   50
 10  \w     78.00 110.00   0.50    4.31    --   97.62-117.00-120.00   64
 11  \w     75.00 100.00   0.50    4.31    --   97.62-153.00-130.00   50
 12  \w     31.00  56.00   0.50    4.31    --   97.62-117.00-120.00   50
 13  \w     30.00  57.00   0.50    4.31    --   97.62 -50.00-150.00   54
 14  \w     30.00  56.00   0.50    4.31    --   97.62 -50.00-120.00   52
 15  \w     79.00 161.00   0.50    4.31    --   97.62  25.00-150.00  164
 16  \w    137.00 163.00   0.50    4.31    --   97.62  33.00 -90.00   52
 17  \w     90.00 132.00   0.50    4.31    --   97.62  33.00 -90.00   84
 18  \w     79.00 104.00   0.50    1.08    --   42.82 138.00-180.00   50
 19  \w     61.00  90.00   0.50    1.08    --   42.82 153.00 -88.00   58
 20  \w     54.00 112.00   0.50    4.31    --   97.62 153.00 -88.00  116
 21  \w     23.00  82.00   0.50    1.08    --   42.82  54.00  90.00  118
 22  \w    102.00 128.00   0.50    4.31    --   97.62 121.00 112.00   52
 23  \w     18.00  43.00   0.50    1.08    --   42.82 -43.00  60.00   50
 24  \w     13.00  71.00   0.50    1.08    --   42.82-121.00  28.00  116
 25  \w     36.00 125.00   0.50    4.31    --   97.62-144.00  30.00  178
 26  \w     30.00  55.00   0.50    4.31    --   97.62 -50.00 150.00   50
 27  \w     30.00  55.00   0.50    4.31    --   97.62 -50.00  60.00   50
 28  \w     -3.00  23.00   0.50    1.08    --   42.82 -43.00 -60.00   52
 29  \w    -61.00 -36.00   0.50    1.08    --  -40.95 -77.00-150.00   50
 30  \w   -106.00 -81.00   0.50    1.08    --  -40.95-153.00-130.00   50
 31  \w   -111.00 -86.00   0.50    1.08    --  -40.95 -77.00-150.00   50
 32  \w   -133.00-108.00   0.50    4.31    --  -95.74-153.00-130.00   50
 33  \w   -145.00 -71.00   0.50    4.31    --  -95.74 -68.00 -60.00  148
 34  \w    -57.00 -31.00   0.50    4.31    --  -95.74  50.00-180.00   52
 35  \w    -54.00 -29.00   0.50    4.31    --  -95.74  50.00-120.00   50
 36  \w    -73.00 -28.00   0.50    1.08    --  -40.95 104.00 -60.00   90
 37  \w    -53.00 -28.00   0.50    4.31    --  -95.74  50.00  60.00   50
 38  \w    -57.00 -31.00   0.50    4.31    --  -95.74  50.00  90.00   52
 39  \w    -68.00 -29.00   0.50    4.31    --  -95.74  68.00 120.00   78
 40  \w    -74.00 -49.00   0.50    1.08    --  -40.95 121.00 112.00   50
 41  \w    -93.00 -68.00   0.50    4.31    --  -95.74 121.00 112.00   50
 42  \w   -106.00 -64.00   0.50    4.31    --  -95.74  96.00 -60.00   84
 43  \w   -103.00 -78.00   0.50    4.31    --  -95.74 153.00 -88.00   50
 44  \w   -104.00 -78.00   0.50    4.31    --  -95.74  96.00-180.00   52
 45  \w    -93.00 -68.00   0.50    1.08    --  -40.95 153.00 -88.00   50
 46  \w    -24.00   1.00   0.50    1.08    --   42.82 -21.00 120.00   50
 47  \w    -95.00 -70.00   0.50    1.08    --  -40.95-138.00 120.00   50
 48  \w   -167.00-139.00   0.50    4.31    --  -95.74 -25.00-150.00   56
;
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24220
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.326
_diffrn_reflns_theta_min         3.098
_exptl_absorpt_coefficient_mu    10.887
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22586
_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    1.689
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.354
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         7640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0596P)^2^+26.2014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6033
_reflns_number_total             7640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02639f2.cif
_cod_data_source_block           co_02_br
_cod_depositor_comments
;

2024-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C35 H62 Br4 Co2 N10 O'
_cod_original_formula_weight         1076.44
_cod_original_formula_moiety         '2(C17 H29 Br Co N5), C H4 O, 2(Br)'
_cod_original_formula_units_Z            4
_cod_database_code               7714472
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.547
_shelx_estimated_absorpt_t_min   0.122
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 O1(H1)
2.b Ternary CH refined with riding coordinates:
 N5(H5), N2(H2), N2A(H2Aa), N5A(H5A)
2.c Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C23(H23a,H23b), C14(H14a,H14b), C12(H12a,H12b), C11(H11a,
 H11b), C6(H6a,H6b), C17(H17a,H17b), C16(H16a,H16b), C9(H9a,H9b), C10(H10a,
 H10b), C34(H34a,H34b), C15(H15a,H15b), C8(H8a,H8b), C24(H24a,H24b), C7(H7a,
 H7b), C27(H27a,H27b), C28(H28a,H28b), C26(H26a,H26b), C29(H29a,H29b), C25(H25a,
 H25b), C30(H30a,H30b), C31(H31a,H31b), C33(H33a,H33b), C32(H32a,H32b)
2.d Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C19(H19), C4(H4), C2(H2a), C3(H3)
2.e Idealised Me refined as rotating group:
 C35(H35a,H35b,H35c)
;
_shelx_res_checksum              15289
_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
;