Luminescent Iridium(III) Complexes Supported by a Tetradentate Trianionic Ligand Scaffold with Mixed O, N, and C Donor Atoms: Synthesis, Structures, Photophysical Properties, and Material Applications
Chen, Daqing; Li, Kai; Guan, Xiangguo; Cheng, Gang; Yang, Chen; Che, Chi-Ming; Organometallics 36 (2017) 1331–; doi:10.1021/acs.organomet.7b00038

data_4089221
_publ_section_title
;
 Luminescent Iridium(III) Complexes Supported by a Tetradentate Trianionic
 Ligand Scaffold with Mixed O, N, and C Donor Atoms: Synthesis,
 Structures, Photophysical Properties, and Material Applications
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1331
_journal_paper_doi               10.1021/acs.organomet.7b00038
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C40 H30 Ir N3 O2, C H Cl3'
_chemical_formula_sum            'C41 H31 Cl3 Ir N3 O2'
_chemical_formula_weight         896.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P -2ac -2n'
_space_group_name_H-M_alt        'P n 21 a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5975(7)
_cell_length_b                   12.4727(6)
_cell_length_c                   17.9014(8)
_cell_measurement_reflns_used    9706
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.63
_cell_measurement_theta_min      3.76
_cell_volume                     3482.6(3)
_computing_cell_refinement       'SADABS V2008/1 (Bruker AXS)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            65777
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        66.514
_diffrn_reflns_theta_max         66.514
_diffrn_reflns_theta_min         3.759
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.872
_exptl_absorpt_correction_T_max  0.6935
_exptl_absorpt_correction_T_min  0.5056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_recrystallization_method CHCl3/Hexane
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 2184 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.088(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5599
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0327P)^2^+2.0858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.754
_reflns_Friedel_fraction_full    0.827
_reflns_Friedel_fraction_max     0.827
_reflns_number_gt                5368
_reflns_number_total             5599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00038_si_002.cif
_cod_data_source_block           david29a_0m
_cod_database_code               4089221
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.506
_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 Ternary CH refined with riding coordinates:
 C41(H41)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C13(H13), C14(H14),
 C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 C35(H35), C36(H36), C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              60120
_shelx_hkl_checksum              48828
_olex2_submission_special_instructions 'No special instructions were received'