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_7716589
_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
'C25 H20 Co N7 O2, Cl0.964 O4, Cl O4, 1.394(H2 O)'
_chemical_formula_sum            'C25 H22.79 Cl1.97 Co N7 O11.4'
_chemical_formula_weight         732.20
_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     dual
_audit_creation_date             2024-07-05
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-06 deposited with the CCDC.	2024-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                97.658(2)
_cell_angle_beta                 108.587(2)
_cell_angle_gamma                107.640(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0838(2)
_cell_length_b                   12.5241(2)
_cell_length_c                   13.9453(2)
_cell_measurement_reflns_used    12423
_cell_measurement_temperature    105.5(5)
_cell_measurement_theta_max      72.3390
_cell_measurement_theta_min      3.4430
_cell_volume                     1385.88(5)
_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    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105.5(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_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    -19.00  34.00   0.50    0.25    --  -47.23  19.00 -30.00  106
  2  \w    -14.00  32.00   0.50    0.25    --  -47.23  19.00  90.00   92
  3  \w    -44.00 -18.00   0.50    0.25    --  -47.23 108.00 153.00   52
  4  \w    -26.00  10.00   0.50    0.25    --  -47.23  19.00-150.00   72
  5  \w    -60.00 -30.00   0.50    0.25    --  -47.23 -57.00-180.00   60
  6  \w   -113.00 -71.00   0.50    1.00    --  -90.25 -45.00 -30.00   84
  7  \w   -122.00 -94.00   0.50    1.00    --  -90.25-108.00  56.00   56
  8  \w   -119.00 -20.00   0.50    0.25    --  -47.23 -77.00  60.00  198
  9  \w   -101.00 -75.00   0.50    1.00    --  -90.25 -30.00  90.00   52
 10  \w    -47.00 -21.00   0.50    1.00    --  -90.25  45.00  90.00   52
 11  \w    -43.00 -18.00   0.50    1.00    --  -90.25  45.00  60.00   50
 12  \w    -50.00 -23.00   0.50    1.00    --  -90.25  45.00   0.00   54
 13  \w    -44.00 -13.00   0.50    1.00    --  -90.25  45.00 -30.00   62
 14  \w    -70.00 -17.00   0.50    1.00    --  -90.25  61.00-180.00  106
 15  \w   -117.00 -92.00   0.50    0.25    --  -47.23 -57.00-180.00   50
 16  \w   -169.00 -70.00   0.50    1.00    --  -90.25 -30.00-180.00  198
 17  \w   -165.00-120.00   0.50    1.00    --  -90.25 -45.00 -30.00   90
 18  \w   -124.00 -84.00   0.50    0.25    --  -47.23-125.00  90.00   80
 19  \w   -163.00-105.00   0.50    1.00    --  -90.25 -61.00 120.00  116
 20  \w   -171.00-119.00   0.50    1.00    --  -90.25 -30.00  90.00  104
 21  \w   -100.00 -41.00   0.50    1.00    --  -90.25  77.00  30.00  118
 22  \w    -81.00 -49.00   0.50    0.25    --  -47.23 108.00 153.00   64
 23  \w    -48.00 -23.00   0.50    1.00    --  -90.25 108.00 153.00   50
 24  \w     31.00  56.00   0.50    0.25    --   47.23-108.00  56.00   50
 25  \w     68.00  99.00   0.50    1.00    --   97.33-108.00  56.00   62
 26  \w     78.00 104.00   0.50    1.00    --   97.33 -95.00  60.00   52
 27  \w     54.00 109.00   0.50    1.00    --   97.33-111.00  30.00  110
 28  \w     69.00  95.00   0.50    1.00    --   97.33 -95.00 -60.00   52
 29  \w     75.00 101.00   0.50    1.00    --   97.33-111.00-120.00   52
 30  \w     74.00 108.00   0.50    1.00    --   97.33-111.00-180.00   68
 31  \w     39.00  64.00   0.50    1.00    --   97.33 -61.00-150.00   50
 32  \w     23.00  67.00   0.50    1.00    --   97.33-111.00-120.00   88
 33  \w     43.00 104.00   0.50    1.00    --   97.33-111.00 -60.00  122
 34  \w     23.00  48.00   0.50    1.00    --   97.33 -45.00  30.00   50
 35  \w     21.00  50.00   0.50    1.00    --   97.33 -45.00  60.00   58
 36  \w     34.00 100.00   0.50    1.00    --   97.33 -77.00  90.00  132
 37  \w     20.00  96.00   0.50    1.00    --   97.33 -95.00  90.00  152
 38  \w     22.00  49.00   0.50    1.00    --   97.33 -45.00 -30.00   54
 39  \w     21.00  48.00   0.50    1.00    --   97.33 -45.00 -90.00   54
 40  \w     24.00  50.00   0.50    1.00    --   97.33 -45.00-150.00   52
 41  \w     25.00  60.00   0.50    1.00    --   97.33 -61.00 -90.00   70
 42  \w     27.00  56.00   0.50    1.00    --   97.33-111.00-180.00   58
 43  \w     18.00  60.00   0.50    1.00    --   97.33 -95.00  60.00   84
 44  \w     26.00  51.00   0.50    1.00    --   97.33 -45.00  90.00   50
 45  \w    117.00 143.00   0.50    1.00    --   97.33 108.00 153.00   52
 46  \w    109.00 155.00   0.50    1.00    --   97.33 111.00  90.00   92
 47  \w    101.00 134.00   0.50    1.00    --   97.33 178.00   0.00   66
 48  \w     97.00 138.00   0.50    1.00    --   97.33 178.00 -60.00   82
 49  \w     63.00  88.00   0.50    1.00    --   97.33 178.00 -60.00   50
;
_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      -0.1017474000
_diffrn_orient_matrix_UB_12      0.0677682000
_diffrn_orient_matrix_UB_13      0.0297848000
_diffrn_orient_matrix_UB_21      -0.1287670000
_diffrn_orient_matrix_UB_22      -0.0440507000
_diffrn_orient_matrix_UB_23      -0.1134873000
_diffrn_orient_matrix_UB_31      -0.1004468000
_diffrn_orient_matrix_UB_32      -0.1062149000
_diffrn_orient_matrix_UB_33      0.0275329000
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18024
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.468
_diffrn_reflns_theta_min         3.458
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80828
_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    1.755
_exptl_crystal_description       needle
_exptl_crystal_F_000             747
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         5271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0264P)^2^+1.1728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5087
_reflns_number_total             5271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01579g2.cif
_cod_data_source_block           fi-014
_cod_depositor_comments
'Adding full bibliography for 7716587--7716594.cif.'
_cod_original_cell_volume        1385.87(5)
_cod_original_formula_sum        'C25 H22.79 Cl1.97 Co N7 O11.40'
_cod_database_code               7716589
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C25 H20 N7 Co O3'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O12)=Sof(H12A)=Sof(H12B)=FVAR(1)
3.a Free rotating group:
 O12(H12A,H12B)
3.b Ternary CH refined with riding coordinates:
 C4(H4), C5(H5)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C7(H7), C22(H22), C25(H25),
 C15(H15), C12(H12), C18(H18), C19(H19), C14(H14), C23(H23), C24(H24), C20(H20),
  C17(H17), C13(H13)
;
_shelx_res_checksum              76493
_shelx_hkl_checksum              97513
_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 1.323
_oxdiff_exptl_absorpt_empirical_full_min 0.836