Synthesis and biological evaluation of mixed-ligands cyclometalated iridium(III)-quinoline complexes
Yang, Yan; Wang, Cheng-Ming; Pan, Feng-Hua; Qin, Qi-Pin; Xie, Qiu-Ji; Chen, Qing; Liang, Hong; Dalton Transactions  (2021) –; doi:10.1039/D1DT02416G

data_7708580
_publ_section_title
;
 Synthesis and biological evaluation of mixed-ligands cyclometalated
 iridium(III)-quinoline complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02416G
_journal_year                    2021
_chemical_formula_moiety         'C39 H24 Br2 Ir N3 O'
_chemical_formula_sum            'C39 H24 Br2 Ir N3 O'
_chemical_formula_weight         902.63
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-10 deposited with the CCDC.	2021-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.1807(5)
_cell_length_b                   18.1807(5)
_cell_length_c                   36.8214(13)
_cell_measurement_reflns_used    6025
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2700
_cell_measurement_theta_min      3.6870
_cell_volume                     12170.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0233
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.931
_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     21.00  61.00   1.00   10.00    --   18.63 -99.00-120.00   40
  2  \w    -85.00 -59.00   1.00   10.00    --  -18.94 178.00-120.00   26
  3  \w    -82.00   9.00   1.00   10.00    --  -18.94 -77.00 -30.00   91
  4  \w    -26.00   0.00   1.00   10.00    --  -18.94 -57.00  90.00   26
  5  \w    -46.00  50.00   1.00   10.00    --  -18.94  77.00  90.00   96
  6  \w    -87.00   7.00   1.00   10.00    --  -18.94 -19.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221501000
_diffrn_orient_matrix_UB_12      0.0320167000
_diffrn_orient_matrix_UB_13      0.0008502000
_diffrn_orient_matrix_UB_21      -0.0316185000
_diffrn_orient_matrix_UB_22      -0.0213792000
_diffrn_orient_matrix_UB_23      -0.0040015000
_diffrn_orient_matrix_UB_31      -0.0057047000
_diffrn_orient_matrix_UB_32      -0.0059865000
_diffrn_orient_matrix_UB_33      0.0188425000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            46769
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.184
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             6944
_refine_diff_density_max         2.793
_refine_diff_density_min         -1.473
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0545P)^2^+118.3956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4827
_reflns_number_total             7659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02416g2.cif
_cod_data_source_block           15
_cod_original_cell_volume        12170.8(8)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7708580
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 H1 O1 N1'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C36(H36)
;
_shelx_res_checksum              58491
_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 1.333
_oxdiff_exptl_absorpt_empirical_full_min 0.676