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_7714471
_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, 3(H2 O)'
_chemical_formula_sum            'C17 H35 Cl2 Co N5 O3'
_chemical_formula_weight         487.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-03-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-07-06 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                79.8000(10)
_cell_angle_beta                 81.4420(10)
_cell_angle_gamma                88.9580(10)
_cell_formula_units_Z            2
_cell_length_a                   8.51040(10)
_cell_length_b                   10.46290(10)
_cell_length_c                   12.91000(10)
_cell_measurement_reflns_used    15855
_cell_measurement_temperature    276(2)
_cell_measurement_theta_max      71.2180
_cell_measurement_theta_min      3.4990
_cell_volume                     1118.75(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      276(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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   -107.00 -63.00   0.50    0.25    --  -42.75 -71.00  35.00   88
  2  \w     66.00  97.00   0.50    0.25    --   44.00  71.00 166.00   62
  3  \w    -14.00  23.00   0.50    0.25    --   44.00 -71.00  35.00   74
  4  \w    -85.00 -60.00   0.50    0.60    --  -99.89  71.00 166.00   50
  5  \w   -158.00 -77.00   0.50    0.60    --  -99.89 -71.00  35.00  162
  6  \w     79.00 116.00   0.50    0.60    --  101.14  71.00 166.00   74
  7  \w    142.00 167.00   0.50    0.60    --  101.14  71.00 166.00   50
  8  \w     35.00  89.00   0.50    0.60    --  101.14 -71.00  35.00  108
  9  \w    -51.00  -3.00   0.50    0.25    --  -10.00 113.00 146.50   96
 10  \w    -24.00   1.00   0.50    0.25    --   14.00 107.00-125.39   50
 11  \w    -79.00 -19.00   0.50    0.25    --  -26.00 133.00 -21.87  120
 12  \w     -3.00  22.00   0.50    0.25    --   26.00 100.00   3.61   50
 13  \w      3.00  28.00   0.50    0.25    --   34.00  94.00 153.40   50
 14  \w      2.00  27.00   0.50    0.25    --   34.00  97.00-177.80   50
 15  \w      1.00  26.00   0.50    0.25    --   34.00  98.00 102.97   50
 16  \w      2.00  27.00   0.50    0.25    --   34.00  95.00 -66.97   50
 17  \w      2.00  27.00   0.50    0.25    --   34.00  97.00  29.64   50
 18  \w      8.00  37.00   0.50    0.25    --   38.00  92.00 -57.46   58
 19  \w    -41.00 -15.00   0.50    0.25    --  -42.00 -84.00 -43.20   52
 20  \w    -40.00 -14.00   0.50    0.25    --  -42.00 -88.00 -66.95   52
 21  \w     13.00  38.00   0.50    0.25    --   42.00  87.00  90.95   50
 22  \w    -40.00 -15.00   0.50    0.25    --  -42.00 -88.00-136.76   50
 23  \w     14.00  39.00   0.50    0.25    --   42.00  86.00-174.03   50
 24  \w     13.00  38.00   0.50    0.25    --   42.00  89.00 -49.71   50
 25  \w    -46.00  -2.00   0.50    0.25    --  -42.75  71.00 166.00   88
 26  \w    -96.00 -52.00   0.50    0.25    --  -42.75 138.00 -60.00   88
 27  \w    -94.00 -46.00   0.50    0.25    --  -42.75 138.00-180.00   96
 28  \w    -39.00 -13.00   0.50    0.25    --  -42.75 -89.00 -82.15   52
 29  \w     16.00  41.00   0.50    0.25    --   46.00  90.00-143.30   50
 30  \w     16.00  41.00   0.50    0.25    --   46.00  92.00  23.98   50
 31  \w     16.00  41.00   0.50    0.25    --   46.00  92.00 114.68   50
 32  \w     16.00  41.00   0.50    0.25    --   46.00  90.00 177.74   50
 33  \w     16.00  41.00   0.50    0.25    --   46.00  90.00-124.05   50
 34  \w     16.00  41.00   0.50    0.25    --   46.00  92.00  71.76   50
 35  \w    -55.00 -27.00   0.50    0.25    --  -50.00 -73.00-126.91   56
 36  \w    -69.00 -29.00   0.50    0.25    --  -54.00 -77.00 141.56   80
 37  \w   -117.00 -91.00   0.50    0.25    --  -54.00 -77.00 141.56   52
 38  \w    -59.00 -33.00   0.50    0.25    --  -54.00 -70.00 -98.60   52
 39  \w    -63.00 -30.00   0.50    0.25    --  -54.00 -74.00 -12.55   66
 40  \w    -70.00 -29.00   0.50    0.25    --  -54.00 -77.00  79.16   82
 41  \w    -64.00 -31.00   0.50    0.25    --  -54.00 -73.00-164.78   66
 42  \w    -57.00 -30.00   0.50    0.25    --  -54.00 -74.00 -49.65   54
 43  \w    -61.00 -35.00   0.50    0.25    --  -58.00 -71.00 -35.80   52
 44  \w    -79.00 -33.00   0.50    0.25    --  -58.00 -75.00 178.45   92
 45  \w    -58.00 -33.00   0.50    0.25    --  -58.00 -76.00  52.07   50
 46  \w    -60.00 -34.00   0.50    0.25    --  -58.00 -73.00  31.36   52
 47  \w    -59.00 -33.00   0.50    0.25    --  -58.00 -75.00 -72.23   52
 48  \w    -63.00 -38.00   0.50    0.25    --  -62.00 -77.00-105.85   50
 49  \w    -82.00 -39.00   0.50    0.25    --  -62.00 -71.00 111.16   86
 50  \w    -78.00 -40.00   0.50    0.25    --  -62.00 -69.00 124.06   76
 51  \w    -64.00 -38.00   0.50    0.25    --  -62.00 -72.00  11.15   52
 52  \w   -130.00 -90.00   0.50    0.25    --  -62.00 -71.00 111.16   80
 53  \w   -101.00 -47.00   0.50    0.25    --  -70.00 -75.00   7.60  108
 54  \w   -134.00 -88.00   0.50    0.25    --  -70.00 -77.00-166.56   92
 55  \w    -80.00 -50.00   0.50    0.25    --  -70.00 -77.00-166.56   60
 56  \w    -95.00 -48.00   0.50    0.25    --  -70.00 -77.00-113.98   94
 57  \w    -79.00 -46.00   0.50    0.25    --  -70.00 -75.00  95.99   66
 58  \w   -130.00-105.00   0.50    0.25    --  -70.00 -75.00  95.99   50
 59  \w   -102.00 -76.00   0.50    0.25    --  -70.00 -67.00-155.06   52
 60  \w    -73.00 -48.00   0.50    0.25    --  -70.00 -67.00-155.06   50
 61  \w    -72.00 -45.00   0.50    0.25    --  -70.00 -76.00 -37.78   54
 62  \w   -121.00 -95.00   0.50    0.25    --  -70.00 -76.00 -37.78   52
 63  \w    -79.00 -49.00   0.50    0.60    --  -74.00 -77.00  31.78   60
 64  \w    -85.00 -49.00   0.50    0.60    --  -74.00 -77.00 166.43   72
 65  \w    -94.00 -49.00   0.50    0.60    --  -74.00 -77.00 -44.03   90
 66  \w    -74.00 -49.00   0.50    0.60    --  -74.00 -77.00  77.59   50
 67  \w    -84.00 -53.00   0.50    0.60    --  -78.00 -76.00 -85.73   62
 68  \w    -83.00 -57.00   0.50    0.60    --  -78.00 -65.00  35.13   52
 69  \w    -79.00 -53.00   0.50    0.60    --  -78.00 -76.00  98.04   52
 70  \w   -140.00 -56.00   0.50    0.60    --  -78.00 -75.00 -64.36  168
 71  \w    -79.00 -54.00   0.50    0.60    --  -78.00 -75.00  -3.77   50
 72  \w    -80.00 -55.00   0.50    0.60    --  -78.00 -72.00 171.47   50
 73  \w    -78.00 -53.00   0.50    0.60    --  -78.00 -75.00  63.95   50
 74  \w   -129.00-103.00   0.50    0.60    --  -82.00 -72.00 -15.38   52
 75  \w    -87.00 -58.00   0.50    0.60    --  -82.00 -76.00 156.58   58
 76  \w    -94.00 -58.00   0.50    0.60    --  -82.00 -73.00 112.81   72
 77  \w   -147.00-120.00   0.50    0.60    --  -82.00 -73.00 112.81   54
 78  \w   -138.00-112.00   0.50    0.60    --  -82.00 -76.00 156.58   52
 79  \w    -96.00 -58.00   0.50    0.60    --  -82.00 -72.00 -15.38   76
 80  \w    -97.00 -57.00   0.50    0.60    --  -82.00 -75.00 -50.67   80
 81  \w    -88.00 -61.00   0.50    0.60    --  -82.00 -72.00-118.56   54
 82  \w   -129.00 -57.00   0.50    0.60    --  -82.00 -75.00 134.01  144
 83  \w    -97.00 -57.00   0.50    0.60    --  -82.00 -77.00-136.97   80
 84  \w   -105.00 -62.00   0.50    0.60    --  -86.00 -74.00  18.00   86
 85  \w    -87.00 -62.00   0.50    0.60    --  -86.00 -73.00 161.80   50
 86  \w    -94.00 -65.00   0.50    0.60    --  -86.00 -75.00 -78.48   58
 87  \w   -153.00-122.00   0.50    0.60    --  -86.00 -75.00 -78.48   62
 88  \w    -89.00 -64.00   0.50    0.60    --  -86.00 -68.00  84.04   50
 89  \w   -142.00-116.00   0.50    0.60    --  -86.00 -68.00  84.04   52
 90  \w   -153.00 -61.00   0.50    0.60    --  -86.00 -77.00-152.81  184
 91  \w   -116.00 -61.00   0.50    0.60    --  -86.00 -77.00  40.80  110
 92  \w   -153.00-127.00   0.50    0.60    --  -86.00 -77.00  40.80   52
 93  \w   -100.00 -69.00   0.50    0.60    --  -90.00 -77.00 -18.72   62
 94  \w   -157.00-105.00   0.50    0.60    --  -90.00 -77.00 -18.72  104
 95  \w    -90.00 -65.00   0.50    0.60    --  -90.00 -77.00  -7.07   50
 96  \w    -98.00 -70.00   0.50    0.60    --  -90.00 -64.00  54.46   56
 97  \w   -126.00 -73.00   0.50    0.60    --  -98.00 -76.00 -90.88  106
 98  \w   -158.00 -79.00   0.50    0.60    --  -99.89 -68.00-120.00  158
 99  \w   -103.00 -78.00   0.50    0.60    --  -99.89 -68.00-180.00   50
100  \w   -166.00 -87.00   0.50    0.60    --  -99.89 -68.00 104.56  158
101  \w   -105.00 -59.00   0.50    0.60    --  -99.89  96.00-150.00   92
102  \w   -119.00 -80.00   0.50    0.60    --  -99.89 -68.00-150.00   78
103  \w   -147.00-121.00   0.50    0.60    --  -99.89 -68.00-150.00   52
104  \w   -166.00 -81.00   0.50    0.60    --  -99.89 -68.00  60.00  170
105  \w    -62.00 -36.00   0.50    0.60    --  -99.89 112.00  11.77   52
106  \w   -109.00 -82.00   0.50    0.60    --  -99.89 112.00  11.77   54
107  \w   -111.00 -85.00   0.50    0.60    --  -99.89-117.00 150.00   52
108  \w   -160.00-105.00   0.50    0.60    --  -99.89-145.00-120.00  110
109  \w   -114.00 -75.00   0.50    0.60    --  -99.89 -77.00 -57.12   78
110  \w   -166.00-135.00   0.50    0.60    --  -99.89 -77.00 -57.12   62
111  \w   -164.00 -75.00   0.50    0.60    --  -99.89 -77.00  90.00  178
112  \w   -157.00 -75.00   0.50    0.60    --  -99.89 -75.00  22.87  164
113  \w   -103.00 -75.00   0.50    0.60    --  -99.89 -77.00   0.00   56
114  \w   -150.00-118.00   0.50    0.60    --  -99.89 -77.00   0.00   64
115  \w   -164.00-101.00   0.50    0.60    --  -99.89 -33.00 -60.00  126
116  \w   -164.00 -76.00   0.50    0.60    --  -99.89 -77.00 150.00  176
117  \w     81.00 110.00   0.50    0.60    --  101.14  68.00 -90.00   58
118  \w    132.00 157.00   0.50    0.60    --  101.14  68.00-180.00   50
119  \w     79.00 105.00   0.50    0.60    --  101.14  68.00-180.00   52
120  \w     77.00 129.00   0.50    0.60    --  101.14  77.00-120.00  104
121  \w     78.00 119.00   0.50    0.60    --  101.14  77.00 -60.00   82
122  \w     75.00 104.00   0.50    0.60    --  101.14-117.00  90.00   58
123  \w     35.00  62.00   0.50    0.60    --  101.14 -68.00 150.00   54
124  \w     65.00 126.00   0.50    0.60    --  101.14-145.00  30.00  122
125  \w    101.00 149.00   0.50    0.60    --  101.14  96.00  90.00   96
126  \w     77.00 122.00   0.50    0.60    --  101.14  77.00 -30.00   90
127  \w     51.00  77.00   0.50    0.60    --  101.14-117.00-120.00   52
128  \w     37.00 109.00   0.50    0.60    --  101.14-117.00 150.00  144
129  \w     37.00  97.00   0.50    0.60    --  101.14 -77.00-180.00  120
130  \w    114.00 164.00   0.50    0.60    --  101.14  68.00 -90.00  100
131  \w     34.00  64.00   0.50    0.60    --  101.14 -59.00-150.00   60
132  \w     44.00  95.00   0.50    0.60    --  101.14-117.00 -60.00  102
133  \w     82.00 141.00   0.50    0.60    --  101.14  68.00 150.00  118
134  \w    139.00 164.00   0.50    0.60    --  101.14  68.00  60.00   50
135  \w     38.00  81.00   0.50    0.60    --  101.14 -68.00 120.00   86
136  \w     81.00 107.00   0.50    0.60    --  101.14  68.00  60.00   52
137  \w     38.00  64.00   0.50    0.60    --  101.14 -59.00  60.00   52
138  \w    126.00 162.00   0.50    0.60    --  101.14  68.00-150.00   72
139  \w     37.00  65.00   0.50    0.60    --  101.14 -59.00 -60.00   56
140  \w     76.00 169.00   0.50    0.60    --  101.14  77.00 120.00  186
141  \w     52.00  82.00   0.50    0.60    --  101.14-117.00  60.00   60
142  \w     83.00 109.00   0.50    0.60    --  101.14  68.00-150.00   52
143  \w     85.00 110.00   0.50    0.60    --  101.14-117.00-120.00   50
144  \w     37.00  71.00   0.50    0.60    --  101.14 -68.00 -90.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1269002000
_diffrn_orient_matrix_UB_12      0.1042700000
_diffrn_orient_matrix_UB_13      -0.0216032000
_diffrn_orient_matrix_UB_21      0.0341784000
_diffrn_orient_matrix_UB_22      0.0584939000
_diffrn_orient_matrix_UB_23      0.0958816000
_diffrn_orient_matrix_UB_31      0.1274428000
_diffrn_orient_matrix_UB_32      0.0899420000
_diffrn_orient_matrix_UB_33      -0.0732808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26262
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.740
_diffrn_reflns_theta_min         3.517
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       prism
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0058(3)
_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   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4329
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0356P)^2^+0.3997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4141
_reflns_number_total             4329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02639f2.cif
_cod_data_source_block           co_01b_cl
_cod_database_code               7714471
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Co  Cl'
_shelx_estimated_absorpt_t_max   0.444
_shelx_estimated_absorpt_t_min   0.239
_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 O(H,H) groups
2. Restrained distances
 O1-H1A = O1-H1B
 0.85 with sigma of 0.02
 H1A-H1B
 1.34 with sigma of 0.04
3.a Free rotating group:
 O3(H3A,H3B), O2(H2B,H2C)
3.b Ternary CH refined with riding coordinates:
 N5(H5), N2(H2)
3.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C16(H16A,H16B), C6(H6A,H6B), C14(H14A,H14B), C13(H13A,H13B),
 C12(H12A,H12B), C15(H15A,H15B), C11(H11A,H11B), C7(H7A,H7B), C10(H10A,H10B),
 C9(H9A,H9B), C8(H8A,H8B)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C4(H4), C3(H3)
;
_shelx_res_checksum              56992
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.886
_oxdiff_exptl_absorpt_empirical_full_min 0.690