Co(III) complexes of the pentadentate NHC ligand PY4Im: carbene-induced <i>trans</i> influences and the non-disappearing <sup>13</sup>C NMR peak.
Ismael, Fouad; Fleming, Cassandra L.; Christopher, Timothy D.; Söhnel, Tilo; Zhou, Yuchen; Krenske, Elizabeth H.; Gahan, Lawrence R.; Blackman, Allan G.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12688–12697; doi:10.1039/d4dt01579g

data_7716587
_publ_section_title
;
 Co(III) complexes of the pentadentate NHC ligand PY4Im: carbene-induced
 <i>trans</i> influences and the non-disappearing <sup>13</sup>C NMR peak.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12688
_journal_page_last               12697
_journal_paper_doi               10.1039/d4dt01579g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C26 H20 Co N6 O3, Cl O4, 2(H2 O)'
_chemical_formula_sum            'C26 H24 Cl Co N6 O9'
_chemical_formula_weight         658.89
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2024-06-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-18 deposited with the CCDC.	2024-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                98.3430(10)
_cell_angle_beta                 110.8070(10)
_cell_angle_gamma                92.9920(10)
_cell_formula_units_Z            2
_cell_length_a                   9.26770(10)
_cell_length_b                   12.22350(10)
_cell_length_c                   12.65450(10)
_cell_measurement_reflns_used    12457
_cell_measurement_temperature    104.5(9)
_cell_measurement_theta_max      72.1850
_cell_measurement_theta_min      3.6750
_cell_volume                     1317.51(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104.5(9)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.994
_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    -33.00  -6.00   0.50    0.40    --  -47.23  69.00 115.00   54
  2  \w    -44.00 -15.00   0.50    1.60    --  -90.25  45.00 120.00   58
  3  \w    -43.00 -12.00   0.50    1.60    --  -90.25  45.00  90.00   62
  4  \w    -67.00 -41.00   0.50    0.40    --  -47.23  69.00 115.00   52
  5  \w    -83.00 -16.00   0.50    1.60    --  -90.25  69.00 115.00  134
  6  \w    -70.00 -23.00   0.50    1.60    --  -90.25  61.00 150.00   94
  7  \w    -55.00 -23.00   0.50    0.40    --  -47.23 -69.00 -16.00   64
  8  \w    -23.00  35.00   0.50    0.40    --  -47.23  19.00 -90.00  116
  9  \w    -44.00 -12.00   0.50    1.60    --  -90.25  45.00 -30.00   64
 10  \w    -58.00 -27.00   0.50    1.60    --  -90.25  61.00 -60.00   62
 11  \w    -45.00 -19.00   0.50    1.60    --  -90.25  45.00-120.00   52
 12  \w    -47.00 -17.00   0.50    1.60    --  -90.25  61.00-180.00   60
 13  \w   -120.00 -63.00   0.50    0.40    --  -47.23 -69.00 -16.00  114
 14  \w     28.00  74.00   0.50    0.40    --   47.23  69.00 115.00   92
 15  \w     86.00 121.00   0.50    1.60    --   97.33  69.00 115.00   70
 16  \w    107.00 159.00   0.50    1.60    --   97.33 111.00  60.00  104
 17  \w    101.00 143.00   0.50    1.60    --   97.33 178.00 120.00   84
 18  \w     67.00  93.00   0.50    1.60    --   97.33 178.00 120.00   52
 19  \w    -32.00  27.00   0.50    0.40    --   47.23 -19.00   0.00  118
 20  \w    -17.00   9.00   0.50    0.40    --   47.23 -69.00 -16.00   52
 21  \w     30.00  55.00   0.50    1.60    --   97.33 -69.00 -16.00   50
 22  \w     65.00 108.00   0.50    1.60    --   97.33-111.00   0.00   86
 23  \w     55.00  98.00   0.50    1.60    --   97.33-111.00  60.00   86
 24  \w     80.00 106.00   0.50    1.60    --   97.33-111.00 120.00   52
 25  \w     74.00 108.00   0.50    1.60    --   97.33-111.00  90.00   68
 26  \w     25.00  69.00   0.50    1.60    --   97.33 -61.00 -60.00   88
 27  \w     50.00 109.00   0.50    1.60    --   97.33-111.00 -90.00  118
 28  \w     60.00 109.00   0.50    1.60    --   97.33-111.00-180.00   98
 29  \w     66.00 105.00   0.50    1.60    --   97.33 -95.00-180.00   78
 30  \w     51.00  82.00   0.50    1.60    --   97.33 -77.00-180.00   62
 31  \w     21.00  51.00   0.50    1.60    --   97.33 -45.00-180.00   60
 32  \w     22.00  47.00   0.50    1.60    --   97.33 -45.00-120.00   50
 33  \w     18.00  60.00   0.50    1.60    --   97.33 -95.00-180.00   84
 34  \w     19.00 104.00   0.50    1.60    --   97.33 -95.00 -90.00  170
 35  \w     20.00  50.00   0.50    1.60    --   97.33 -45.00 -30.00   60
 36  \w     21.00  50.00   0.50    1.60    --   97.33 -45.00   0.00   58
 37  \w     25.00  51.00   0.50    1.60    --   97.33-111.00  90.00   52
 38  \w     24.00  66.00   0.50    1.60    --   97.33-111.00 120.00   84
 39  \w     22.00  51.00   0.50    1.60    --   97.33 -45.00 150.00   58
 40  \w   -121.00 -32.00   0.50    0.40    --  -47.23 -57.00 150.00  178
 41  \w   -128.00 -83.00   0.50    1.60    --  -90.25 -69.00 -16.00   90
 42  \w   -126.00 -83.00   0.50    1.60    --  -90.25 -95.00  90.00   86
 43  \w   -173.00 -60.00   0.50    1.60    --  -90.25 -15.00 150.00  226
 44  \w   -118.00 -60.00   0.50    1.60    --  -90.25 -15.00-150.00  116
 45  \w   -171.00-145.00   0.50    1.60    --  -90.25 -15.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1374449000
_diffrn_orient_matrix_UB_12      0.0676228000
_diffrn_orient_matrix_UB_13      -0.0056434000
_diffrn_orient_matrix_UB_21      0.0479279000
_diffrn_orient_matrix_UB_22      0.0739311000
_diffrn_orient_matrix_UB_23      -0.0734589000
_diffrn_orient_matrix_UB_31      -0.1041006000
_diffrn_orient_matrix_UB_32      -0.0799624000
_diffrn_orient_matrix_UB_33      -0.1098664000
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16035
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.729
_diffrn_reflns_theta_min         5.138
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.644
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.00059(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         4733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0369P)^2^+0.5289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4561
_reflns_number_total             4733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01579g2.cif
_cod_data_source_block           fi-005
_cod_depositor_comments
'Adding full bibliography for 7716587--7716594.cif.'
_cod_database_code               7716587
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C25 H20 Co N6 C O3'
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.416
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4), C5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C20(H20), C2(H2), C9(H9), C22(H22), C8(H8), C24(H24), C23(H23),
 C7(H7), C25(H25), C18(H18), C3(H3), C17(H17), C19(H19), C14(H14), C15(H15),
 C13(H13), C12(H12)
;
_shelx_res_checksum              81428
_shelx_hkl_checksum              8151
_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 5.095
_oxdiff_exptl_absorpt_empirical_full_min 0.447