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_7715878
_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         'C38 H26 Ir N6, Cl, 1.5[C4H10O]'
_chemical_formula_sum            'C44 H41 Cl Ir N6 O1.5'
_chemical_formula_weight         905.48
_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     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                 112.536(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9468(6)
_cell_length_b                   13.8283(2)
_cell_length_c                   24.2672(5)
_cell_measurement_reflns_used    26266
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      68.2170
_cell_measurement_theta_min      3.4750
_cell_volume                     8042.2(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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_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   -103.00 -32.00   0.50    0.50    --  -38.50 -32.00  81.00  142
  2  \w    -45.00  26.00   0.50    0.50    --  -38.50  32.00-119.00  142
  3  \w    -21.00  50.00   0.50    0.50    --   43.40 -32.00  81.00  142
  4  \w     37.00 108.00   0.50    0.50    --   43.40  32.00-119.00  142
  5  \w     29.00 100.00   0.50    2.00    --   93.53 -32.00  81.00  142
  6  \w     87.00 158.00   0.50    2.00    --   93.53  32.00-119.00  142
  7  \w    -45.00  30.00   0.50    0.50    --  -38.50  21.00 -30.00  150
  8  \w   -107.00 -32.00   0.50    0.50    --  -38.50 -21.00   0.00  150
  9  \w    -45.00  26.00   0.50    0.50    --  -38.50  32.00  90.00  142
 10  \w    -29.00  58.00   0.50    0.50    --   43.40 -11.00 -90.00  174
 11  \w      8.00  78.00   0.50    0.50    --   43.40-104.00  60.00  140
 12  \w     35.00  98.00   0.50    0.50    --   43.40-138.00-180.00  126
 13  \w     32.00 105.00   0.50    0.50    --   43.40  43.00 120.00  146
 14  \w     89.00 160.00   0.50    2.00    --   93.53  25.00-180.00  142
 15  \w    104.00 157.00   0.50    2.00    --   93.53  77.00 -30.00  106
 16  \w    104.00 157.00   0.50    2.00    --   93.53  77.00  30.00  106
 17  \w    102.00 157.00   0.50    2.00    --   93.53 117.00  90.00  110
 18  \w     32.00 106.00   0.50    2.00    --   93.53 -42.00 -30.00  148
 19  \w     27.00  98.00   0.50    2.00    --   93.53 -25.00 -90.00  142
 20  \w     89.00 160.00   0.50    2.00    --   93.53  25.00  90.00  142
 21  \w     25.00 106.00   0.50    2.00    --   93.53 -96.00   0.00  162
 22  \w    104.00 157.00   0.50    2.00    --   93.53  77.00-180.00  106
 23  \w    104.00 157.00   0.50    2.00    --   93.53  77.00 -90.00  106
 24  \w    104.00 157.00   0.50    2.00    --   93.53  77.00   0.00  106
 25  \w     30.00 116.00   0.50    2.00    --   93.53 -77.00  30.00  172
 26  \w     87.00 156.00   0.50    2.00    --   93.53 145.00  90.00  138
 27  \w    102.00 157.00   0.50    2.00    --   93.53 117.00-120.00  110
 28  \w     38.00 126.00   0.50    2.00    --   93.53-145.00   0.00  176
 29  \w   -101.00 -19.00   0.50    0.50    --  -38.50 -65.00 150.00  164
 30  \w   -101.00 -31.00   0.50    0.50    --  -38.50 -65.00   0.00  140
 31  \w     25.00 106.00   0.50    0.50    --   43.40  65.00-120.00  162
 32  \w     25.00 106.00   0.50    0.50    --   43.40  65.00  60.00  162
 33  \w     25.00 106.00   0.50    0.50    --   43.40  65.00 -30.00  162
 34  \w     25.00 106.00   0.50    0.50    --   43.40  65.00 -90.00  162
 35  \w      8.00  78.00   0.50    0.50    --   43.40-104.00-150.00  140
 36  \w     25.00 106.00   0.50    0.50    --   43.40  65.00 150.00  162
 37  \w     25.00 106.00   0.50    0.50    --   43.40  65.00 120.00  162
 38  \w     25.00 106.00   0.50    0.50    --   43.40  65.00   0.00  162
 39  \w     25.00 106.00   0.50    0.50    --   43.40  65.00 -60.00  162
;
_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      0.0320987000
_diffrn_orient_matrix_UB_12      -0.0432401000
_diffrn_orient_matrix_UB_13      0.0586190000
_diffrn_orient_matrix_UB_21      -0.0565868000
_diffrn_orient_matrix_UB_22      0.0153142000
_diffrn_orient_matrix_UB_23      0.0124876000
_diffrn_orient_matrix_UB_31      -0.0222008000
_diffrn_orient_matrix_UB_32      -0.1015865000
_diffrn_orient_matrix_UB_33      -0.0230711000
_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  0.0382
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40499
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.481
_diffrn_reflns_theta_min         3.689
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64665
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.09
_refine_diff_density_max         6.877
_refine_diff_density_min         -2.269
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0531
_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^)+(0.1026P)^2^+21.3052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6894
_reflns_number_total             7342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03766e2.cif
_cod_data_source_block           18
_cod_depositor_comments
'Adding full bibliography for 7715878--7715882.cif.'
_cod_original_formula_sum        'C44 H41 Cl Ir N6 O1.50'
_cod_database_code               7715878
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C312 H224 Cl8 Ir8 N72 '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Riding coordinates:
 N17(H17), N31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C18(H18), C26(H26), C32(H32), C37(H37), C38(H38), C39(H39), C40(H40),
 C41(H41), C44(H44), C45(H45), C48(H48), C50(H50), C57(H57), C60(H60), C62(H62),
  C63(H63), C64(H64), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 532 electrons were 
found in a volume of 2646\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[C4H10O] per Asymmetric Unit 
which account for 504 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              81770
_shelx_fab_checksum              91047
_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 3.758
_oxdiff_exptl_absorpt_empirical_full_min 0.620