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_7715879
_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         'C36 H26 Ir N6, Cl, C4 H10 O'
_chemical_formula_sum            'C40 H36 Cl Ir N6 O'
_chemical_formula_weight         844.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-08 deposited with the CCDC.	2024-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.64348(9)
_cell_length_b                   8.66040(4)
_cell_length_c                   22.95688(13)
_cell_measurement_reflns_used    51759
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      69.7260
_cell_measurement_theta_min      3.8250
_cell_volume                     3507.80(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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   -105.00 -21.00   0.50    0.50    --  -38.50 152.00-168.00  168
  2  \w    -84.00  -3.00   0.50    0.50    --  -38.50 121.00  31.00  162
  3  \w     42.00 109.00   0.50    0.50    --   42.60-152.00 149.00  134
  4  \w     25.00  88.00   0.50    0.50    --   42.60-121.00 -50.00  126
  5  \w     33.00 110.00   0.50    2.00    --   96.98-121.00 -50.00  154
  6  \w    100.00 161.00   0.50    2.00    --   96.98 121.00  31.00  122
  7  \w     42.00 130.00   0.50    2.00    --   96.98-152.00 149.00  176
  8  \w   -103.00 -16.00   0.50    0.50    --  -38.50 -72.00-172.31  174
  9  \w   -108.00 -28.00   0.50    0.50    --  -38.50 -21.00  60.00  160
 10  \w    -52.00  24.00   0.50    0.50    --  -38.50  43.00-120.00  152
 11  \w   -101.00 -21.00   0.50    0.50    --  -38.50 -54.00 -30.00  160
 12  \w    -52.00  24.00   0.50    0.50    --  -38.50  43.00  30.00  152
 13  \w    -47.00  27.00   0.50    0.50    --  -38.50  32.00  90.00  148
 14  \w   -102.00 -17.00   0.50    0.50    --  -38.50 -69.00 131.32  170
 15  \w   -104.00 -30.00   0.50    0.50    --  -38.50 -32.00-120.00  148
 16  \w    -20.00  68.00   0.50    0.50    --   42.60 -77.00 -60.00  176
 17  \w     20.00 107.00   0.50    0.50    --   42.60  74.00  79.70  174
 18  \w     -8.00  71.00   0.50    0.50    --   42.60 -89.00 150.00  158
 19  \w     34.00 108.00   0.50    0.50    --   42.60  32.00-120.00  148
 20  \w    -20.00  56.00   0.50    0.50    --   42.60 -43.00 -30.00  152
 21  \w     34.00 108.00   0.50    0.50    --   42.60  32.00 150.00  148
 22  \w     35.00  98.00   0.50    0.50    --   42.60-138.00 -60.00  126
 23  \w     38.00 126.00   0.50    2.00    --   96.98-145.00 -60.00  176
 24  \w     27.00 105.00   0.50    2.00    --   96.98 -96.00  60.00  156
 25  \w     87.00 161.00   0.50    2.00    --   96.98 145.00 -30.00  148
 26  \w     31.00 125.00   0.50    2.00    --   96.98 -87.00 -60.00  188
 27  \w     31.00 125.00   0.50    2.00    --   96.98 -87.00  90.00  188
 28  \w     88.00 162.00   0.50    2.00    --   96.98  33.00   0.00  148
 29  \w     84.00 160.00   0.50    2.00    --   96.98  42.00  90.00  152
 30  \w     32.00 106.00   0.50    2.00    --   96.98 -33.00 120.00  148
 31  \w    105.00 167.00   0.50    2.00    --   96.98  96.00 -90.00  124
 32  \w     83.00 168.00   0.50    2.00    --   96.98  17.00-120.00  170
 33  \w     34.00 110.00   0.50    2.00    --   96.98 -42.00-180.00  152
 34  \w    102.00 162.00   0.50    2.00    --   96.98 117.00-180.00  120
 35  \w     34.00 116.00   0.50    2.00    --   96.98 -59.00  90.00  164
 36  \w    104.00 162.00   0.50    2.00    --   96.98  77.00  30.00  116
 37  \w     34.00 116.00   0.50    2.00    --   96.98 -59.00 -90.00  164
 38  \w     32.00 109.00   0.50    2.00    --   96.98-117.00 150.00  154
 39  \w     27.00 105.00   0.50    2.00    --   96.98 -96.00 120.00  156
 40  \w     87.00 161.00   0.50    2.00    --   96.98 145.00 -90.00  148
 41  \w     38.00 126.00   0.50    2.00    --   96.98-145.00  90.00  176
 42  \w     34.00 110.00   0.50    2.00    --   96.98 -42.00 -90.00  152
 43  \w     27.00 105.00   0.50    2.00    --   96.98 -96.00 -90.00  156
 44  \w     29.00 106.00   0.50    2.00    --   96.98 -25.00-150.00  154
 45  \w     81.00 160.00   0.50    2.00    --   96.98  50.00 -60.00  158
 46  \w    102.00 162.00   0.50    2.00    --   96.98 117.00-120.00  120
 47  \w     88.00 162.00   0.50    2.00    --   96.98  33.00  30.00  148
 48  \w     74.00 161.00   0.50    2.00    --   96.98  72.00 -38.28  174
 49  \w     82.00 161.00   0.50    2.00    --   96.98 152.00-168.00  158
 50  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -73.00-100.23  176
 51  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -73.00  23.30  176
 52  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -74.00 133.77  176
 53  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -73.00 166.35  176
 54  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -74.00 -10.02  176
 55  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -74.00 100.18  176
 56  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -74.00  77.72  176
 57  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -74.00 -58.05  176
 58  \w   -102.00 -17.00   0.50    0.50    --  -38.50 -67.00-140.49  170
 59  \w   -103.00 -16.00   0.50    0.50    --  -38.50 -72.00  49.43  174
 60  \w     19.00 107.00   0.50    0.50    --   42.60  73.00-163.67  176
 61  \w     19.00 116.00   0.50    0.50    --   42.60  11.00-150.00  194
 62  \w     21.00 107.00   0.50    0.50    --   42.60  69.00-125.69  172
 63  \w     22.00 106.00   0.50    0.50    --   42.60  65.00  60.00  168
 64  \w     22.00 106.00   0.50    0.50    --   42.60  65.00 150.00  168
 65  \w    -20.00  56.00   0.50    0.50    --   42.60 -43.00  90.00  152
 66  \w     20.00 107.00   0.50    0.50    --   42.60  74.00 -38.03  174
 67  \w     25.00 106.00   0.50    0.50    --   42.60  54.00 -90.00  162
 68  \w     22.00 106.00   0.50    0.50    --   42.60  65.00  30.00  168
 69  \w     21.00 107.00   0.50    0.50    --   42.60  70.00 -63.30  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68323
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.856
_diffrn_reflns_theta_min         3.851
_exptl_absorpt_coefficient_mu    8.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.313
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 2998 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.028(3)
_refine_ls_extinction_coef       0.000092(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         6486
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+4.2423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                6437
_reflns_number_total             6486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03766e2.cif
_cod_data_source_block           17
_cod_depositor_comments
'Adding full bibliography for 7715878--7715882.cif.'
_cod_database_code               7715879
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.591
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N5(H5), C30(H30), C29(H29), C28(H28), C27(H27), C33(H33), C34(H34),
 C35(H35), C36(H36), C16(H16), C17(H17), C18(H18), C19(H19), C25(H25), C24(H24),
  C23(H23), C22(H22), C4(H4), C5(H5A), C6(H6A), C7(H7), C13(H13), C12(H12),
 C11(H11), C10(H10)
2.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              8979
_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
;