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_7716591
_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 N9, 2(Cl O4), H2 O'
_chemical_formula_sum            'C25 H22 Cl2 Co N9 O9'
_chemical_formula_weight         722.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 116.387(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.5235(3)
_cell_length_b                   12.12400(10)
_cell_length_c                   22.4083(3)
_cell_measurement_reflns_used    17768
_cell_measurement_temperature    105(1)
_cell_measurement_theta_max      72.1950
_cell_measurement_theta_min      4.2260
_cell_volume                     5481.61(15)
_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      105(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.963
_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    -24.00  20.00   0.50    0.48    --  -47.23  19.00  30.00   88
  2  \w    -48.00 -11.00   0.50    1.86    --  -90.25 111.00 -48.00   74
  3  \w    -67.00 -42.00   0.50    0.48    --  -47.23 111.00 -48.00   50
  4  \w    -49.00 -15.00   0.50    1.86    --  -90.25  45.00 150.00   68
  5  \w    -80.00 -54.00   0.50    1.86    --  -90.25 111.00 -48.00   52
  6  \w    -70.00 -37.00   0.50    1.86    --  -90.25  61.00 -60.00   66
  7  \w    -33.00  -4.00   0.50    0.48    --  -47.23  38.00-120.00   58
  8  \w    -50.00 -12.00   0.50    1.86    --  -90.25  45.00-180.00   76
  9  \w   -124.00 -73.00   0.50    0.48    --  -47.23-125.00 -60.00  102
 10  \w   -108.00 -74.00   0.50    0.48    --  -47.23-125.00  30.00   68
 11  \w   -117.00 -83.00   0.50    1.86    --  -90.25-111.00 120.00   68
 12  \w   -165.00-128.00   0.50    1.86    --  -90.25-111.00 120.00   74
 13  \w   -149.00-124.00   0.50    1.86    --  -90.25-111.00-141.00   50
 14  \w   -166.00 -81.00   0.50    1.86    --  -90.25-111.00-150.00  170
 15  \w     57.00  82.00   0.50    0.48    --   47.23-111.00-141.00   50
 16  \w     75.00 108.00   0.50    1.86    --   97.33-111.00 -60.00   66
 17  \w     32.00  58.00   0.50    1.86    --   97.33-111.00 -60.00   52
 18  \w     24.00  74.00   0.50    1.86    --   97.33-111.00-141.00  100
 19  \w     26.00  51.00   0.50    1.86    --   97.33 -45.00-180.00   50
 20  \w     21.00  49.00   0.50    1.86    --   97.33 -45.00-150.00   56
 21  \w     22.00  50.00   0.50    1.86    --   97.33 -45.00 -90.00   56
 22  \w     21.00  46.00   0.50    1.86    --   97.33 -45.00 -60.00   50
 23  \w     23.00  51.00   0.50    1.86    --   97.33 -45.00   0.00   56
 24  \w     23.00  49.00   0.50    1.86    --   97.33 -45.00  60.00   52
 25  \w     29.00  54.00   0.50    1.86    --   97.33 -61.00  30.00   50
 26  \w    -21.00  27.00   0.50    0.48    --   47.23 -19.00 -90.00   96
 27  \w    -31.00  27.00   0.50    0.48    --   47.23 -19.00-180.00  116
 28  \w    115.00 140.00   0.50    1.86    --   97.33 111.00 -48.00   50
 29  \w    148.00 175.00   0.50    1.86    --   97.33 111.00  60.00   54
 30  \w    115.00 140.00   0.50    1.86    --   97.33 178.00 -60.00   50
 31  \w    103.00 145.00   0.50    1.86    --   97.33 178.00 -30.00   84
 32  \w    104.00 141.00   0.50    1.86    --   97.33 178.00  30.00   74
 33  \w    104.00 129.00   0.50    1.86    --   97.33 111.00  60.00   50
 34  \w     73.00  98.00   0.50    1.86    --   97.33 178.00  30.00   50
 35  \w     63.00  88.00   0.50    1.86    --   97.33 178.00 -30.00   50
 36  \w     64.00  90.00   0.50    1.86    --   97.33 178.00 -60.00   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      0.0202539000
_diffrn_orient_matrix_UB_12      -0.0108664000
_diffrn_orient_matrix_UB_13      0.0750744000
_diffrn_orient_matrix_UB_21      -0.0166194000
_diffrn_orient_matrix_UB_22      -0.1239176000
_diffrn_orient_matrix_UB_23      -0.0092364000
_diffrn_orient_matrix_UB_31      0.0717378000
_diffrn_orient_matrix_UB_32      -0.0257514000
_diffrn_orient_matrix_UB_33      0.0129670000
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20952
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.371
_diffrn_reflns_theta_min         4.254
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35920
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00024(3)
_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   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0702P)^2^+8.5424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5061
_reflns_number_total             5213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01579g2.cif
_cod_data_source_block           fi-004
_cod_depositor_comments
'Adding full bibliography for 7716587--7716594.cif.'
_cod_original_cell_volume        5481.60(14)
_cod_database_code               7716591
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C25 H20 Co N9'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C20(H20), C3(H3), C15(H15), C14(H14), C13(H13), C7(H7), C23(H23),
 C12(H12), C9(H9), C8(H8), C10(H10), C18(H18), C24(H24), C19(H19), C17(H17),
 C2(H2), C22(H22)
;
_shelx_res_checksum              72059
_shelx_hkl_checksum              36078
_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 1.691
_oxdiff_exptl_absorpt_empirical_full_min 0.643