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_7715881
_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 H29 Ir N5, Cl, 0.5[[C2H14O5]]'
_chemical_formula_sum            'C37 H36 Cl Ir N5 O2.5'
_chemical_formula_weight         818.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           117
_space_group_name_Hall           'P -4 -2ab'
_space_group_name_H-M_alt        'P -4 b 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-06
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.0735(4)
_cell_length_b                   28.0735(4)
_cell_length_c                   8.9606(2)
_cell_measurement_reflns_used    31604
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      28.2670
_cell_measurement_theta_min      3.4520
_cell_volume                     7062.0(2)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_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    -85.00  12.00   0.50   55.00    --  -11.81 -11.00 -28.00  194
  2  \w    -20.00  58.00   0.50   55.00    --  -11.81  11.00 144.00  156
  3  \w    -54.00 -12.00   0.50   55.00    --   11.89 -11.00 -28.00   84
  4  \w     37.00  62.00   0.50   55.00    --   11.89  11.00 144.00   50
  5  \w    -37.00  14.00   0.50   55.00    --  -11.81 -77.00 120.00  102
  6  \w     -7.00  19.00   0.50   55.00    --  -11.81-108.00 -44.42   52
  7  \w    -75.00 -43.00   0.50   55.00    --  -11.81 -57.00 120.00   64
  8  \w    -34.00  -4.00   0.50   55.00    --  -11.81 -57.00 120.00   60
  9  \w    -37.00   0.00   0.50   55.00    --  -11.81  77.00-120.00   74
 10  \w    -55.00 -29.00   0.50   55.00    --  -11.81 126.00-171.11   52
 11  \w     -4.00  24.00   0.50   55.00    --  -11.81-111.00  44.49   56
 12  \w    -27.00  16.00   0.50   55.00    --  -11.81 -90.00  67.74   86
 13  \w    -23.00  11.00   0.50   55.00    --  -11.81  77.00  30.00   68
 14  \w     -7.00  41.00   0.50   55.00    --  -11.81  19.00 -60.00   96
 15  \w    -52.00  19.00   0.50   55.00    --   11.89 -38.00 -30.00  142
 16  \w    -58.00  24.00   0.50   55.00    --   11.89 -19.00-150.00  164
;
_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      0.0126232000
_diffrn_orient_matrix_UB_12      -0.0019190000
_diffrn_orient_matrix_UB_13      -0.0683073000
_diffrn_orient_matrix_UB_21      -0.0218645000
_diffrn_orient_matrix_UB_22      -0.0030744000
_diffrn_orient_matrix_UB_23      -0.0386939000
_diffrn_orient_matrix_UB_31      -0.0017136000
_diffrn_orient_matrix_UB_32      0.0249714000
_diffrn_orient_matrix_UB_33      -0.0100041000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1938
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            91934
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.417
_diffrn_reflns_theta_min         3.230
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.897
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.464
_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    1.539
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Flack x determined using 2576 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.045(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         8552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0688P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1282
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                6784
_reflns_number_total             8552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03766e2.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 7715878--7715882.cif.'
_cod_original_cell_volume        7062.0(3)
_cod_original_formula_sum        'C37 H36 Cl Ir N5 O2.50'
_cod_database_code               7715881
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H39 Ir1 N5 Cl1 O2.5'
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C19(H19), C26(H26), C22(H22), C27(H27), C12(H12), C17(H17), N5(H5),
 C34(H34), C15(H15), C4(H4), C16(H16), C6(H6), C9(H9), C11(H11), C14(H14),
 C25(H25), C31(H31), C21(H21), C20(H20), C24(H24), C5(H5A), C10(H10)
2.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 252 electrons were 
found in a volume of 1632\%A^3^ in the unit cell. 
This is consistent with the presence of 
1.5[water] and 1 [methanol] molecules per Asymmetric Unit 
which account for 264 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99845
_shelx_fab_checksum              6106
_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 2.070
_oxdiff_exptl_absorpt_empirical_full_min 0.345