Experimental and theoretical studies of pH-responsive iridium(III) complexes of azole and N-heterocyclic carbene ligands.
Hashemzadeh, Tahmineh; Christofferson, Andrew J.; White, Keith F.; Barnard, Peter J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8478–8493; doi:10.1039/d3dt03766e

data_7715882
_publ_section_title
;
 Experimental and theoretical studies of pH-responsive iridium(III)
 complexes of azole and N-heterocyclic carbene ligands.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8478
_journal_page_last               8493
_journal_paper_doi               10.1039/d3dt03766e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C30 H24 Ir N6, C2 H3 N, Cl'
_chemical_formula_sum            'C32 H27 Cl Ir N7'
_chemical_formula_weight         737.25
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.392(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.64190(10)
_cell_length_b                   32.2748(5)
_cell_length_c                   10.5786(2)
_cell_measurement_reflns_used    30824
_cell_measurement_temperature    180(40)
_cell_measurement_theta_max      68.4940
_cell_measurement_theta_min      4.1680
_cell_volume                     2910.98(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 40.53 (release 29-04-2019))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180(40)
_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 0.995
_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     28.00 106.00   0.50    1.00    --   43.40  56.00 111.00  156
  2  \w    -19.00  59.00   0.50    1.00    --   43.40 -56.00 -31.00  156
  3  \w     31.00 110.00   0.50    4.00    --   93.53 -56.00 -31.00  158
  4  \w     78.00 156.00   0.50    4.00    --   93.53  56.00 111.00  156
  5  \w   -102.00 -17.00   0.50    1.00    --  -38.50 -74.00 138.68  170
  6  \w   -101.00 -19.00   0.50    1.00    --  -38.50 -66.00-100.88  164
  7  \w    -54.00  24.00   0.50    1.00    --  -38.50  56.00 111.00  156
  8  \w    -61.00  25.00   0.50    1.00    --  -38.50  77.00-120.00  172
  9  \w    -93.00 -14.00   0.50    1.00    --  -38.50 138.00 -30.00  158
 10  \w   -101.00 -19.00   0.50    1.00    --  -38.50 -65.00 -90.00  164
 11  \w   -101.00 -22.00   0.50    1.00    --  -38.50 -56.00 -31.00  158
 12  \w    -18.00  55.00   0.50    1.00    --   43.40 -43.00 150.00  146
 13  \w     37.00 112.00   0.50    1.00    --   43.40  21.00-120.00  150
 14  \w     37.00 112.00   0.50    1.00    --   43.40  21.00  30.00  150
 15  \w    -21.00  50.00   0.50    1.00    --   43.40 -32.00 -60.00  142
 16  \w      8.00  78.00   0.50    1.00    --   43.40-104.00 150.00  140
 17  \w      8.00  78.00   0.50    1.00    --   43.40-104.00 -30.00  140
 18  \w     38.00 126.00   0.50    4.00    --   93.53-145.00 -30.00  176
 19  \w    104.00 157.00   0.50    4.00    --   93.53  77.00  60.00  106
 20  \w     23.00 102.00   0.50    4.00    --   93.53 -17.00-120.00  158
 21  \w     29.00 121.00   0.50    4.00    --   93.53 -87.00 -30.00  184
 22  \w     87.00 156.00   0.50    4.00    --   93.53 145.00 -90.00  138
 23  \w     38.00 126.00   0.50    4.00    --   93.53-145.00 -60.00  176
 24  \w     27.00  98.00   0.50    4.00    --   93.53 -25.00 -30.00  142
 25  \w     23.00 102.00   0.50    4.00    --   93.53 -17.00  30.00  158
 26  \w     86.00 164.00   0.50    4.00    --   93.53  17.00-150.00  156
 27  \w     25.00 106.00   0.50    4.00    --   93.53 -96.00 -30.00  162
 28  \w     87.00 156.00   0.50    4.00    --   93.53 145.00-150.00  138
 29  \w     25.00 106.00   0.50    4.00    --   93.53 -96.00   0.00  162
 30  \w    104.00 157.00   0.50    4.00    --   93.53  77.00 150.00  106
 31  \w     31.00 111.00   0.50    4.00    --   93.53 -59.00  30.00  160
 32  \w     30.00 109.00   0.50    4.00    --   93.53-117.00 150.00  158
 33  \w     30.00 109.00   0.50    4.00    --   93.53-117.00 -30.00  158
 34  \w     86.00 164.00   0.50    4.00    --   93.53  17.00 -90.00  156
 35  \w    104.00 157.00   0.50    4.00    --   93.53  77.00  30.00  106
 36  \w     30.00 109.00   0.50    4.00    --   93.53-117.00  60.00  158
 37  \w     30.00 101.00   0.50    4.00    --   93.53 -33.00 150.00  142
 38  \w     31.00 114.00   0.50    4.00    --   93.53 -68.00-180.00  166
 39  \w     29.00 121.00   0.50    4.00    --   93.53 -87.00  90.00  184
 40  \w     32.00 106.00   0.50    4.00    --   93.53 -42.00  90.00  148
 41  \w    104.00 157.00   0.50    4.00    --   93.53  77.00   0.00  106
 42  \w    104.00 157.00   0.50    4.00    --   93.53  77.00 -60.00  106
 43  \w     31.00 114.00   0.50    4.00    --   93.53 -68.00 120.00  166
 44  \w   -102.00 -17.00   0.50    1.00    --  -38.50 -73.00-152.42  170
 45  \w   -102.00 -17.00   0.50    1.00    --  -38.50 -74.00  22.00  170
 46  \w   -101.00 -18.00   0.50    1.00    --  -38.50 -70.00  67.88  166
 47  \w   -101.00 -18.00   0.50    1.00    --  -38.50 -70.00 -55.27  166
 48  \w     22.00 107.00   0.50    1.00    --   43.40  72.00-104.10  170
 49  \w     25.00 106.00   0.50    1.00    --   43.40  65.00 150.00  162
 50  \w     28.00 106.00   0.50    1.00    --   43.40  54.00 -60.00  156
 51  \w     23.00 107.00   0.50    1.00    --   43.40  71.00  50.13  168
 52  \w     22.00 107.00   0.50    1.00    --   43.40  72.00 165.18  170
 53  \w    -25.00  50.00   0.50    1.00    --   43.40 -21.00-120.00  150
 54  \w     22.00 107.00   0.50    1.00    --   43.40  74.00  -0.23  170
 55  \w     25.00 106.00   0.50    1.00    --   43.40  65.00 -30.00  162
 56  \w     29.00 116.00   0.50    1.00    --   43.40  11.00 120.00  174
 57  \w     22.00 107.00   0.50    1.00    --   43.40  73.00-145.79  170
 58  \w     74.00 156.00   0.50    4.00    --   93.53  67.00 -21.85  164
 59  \w     74.00 157.00   0.50    4.00    --   93.53  68.00-164.19  166
 60  \w     73.00 157.00   0.50    4.00    --   93.53  70.00  40.63  168
 61  \w     74.00 156.00   0.50    4.00    --   93.53  67.00 139.78  164
 62  \w     77.00 156.00   0.50    4.00    --   93.53  58.00 -70.07  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu 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      0.1285877000
_diffrn_orient_matrix_UB_12      0.0238931000
_diffrn_orient_matrix_UB_13      -0.0547372000
_diffrn_orient_matrix_UB_21      0.0503054000
_diffrn_orient_matrix_UB_22      0.0212250000
_diffrn_orient_matrix_UB_23      0.1309022000
_diffrn_orient_matrix_UB_31      0.1164537000
_diffrn_orient_matrix_UB_32      -0.0354608000
_diffrn_orient_matrix_UB_33      0.0412188000
_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  0.0508
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            53765
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.572
_diffrn_reflns_theta_min         4.452
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.996
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       plank
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.298
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0149P)^2^+21.2145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5319
_reflns_number_total             5339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03766e2.cif
_cod_data_source_block           16
_cod_depositor_comments
'Adding full bibliography for 7715878--7715882.cif.'
_cod_database_code               7715882
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C33 H20 N6 Cl1 Ir1'
_shelx_estimated_absorpt_t_max   0.585
_shelx_estimated_absorpt_t_min   0.137
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C17(H17), C15(H15), C16(H16), C21(H21), C24(H24),
 C27(H27), C8(H8), C18(H18), C13(H13), C20(H20), C6(H6), C5(H5), C29(H29),
 C11(H11), C12(H12), C26(H26), C10(H10), C7(H7), C25(H25)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              58117
_olex2_exptl_crystal_mounting_method
'A crystal was selected from its mother liqor, coated in protective oil and mounted on a nylon loop.'
_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 3.889
_oxdiff_exptl_absorpt_empirical_full_min 0.696