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_4089226
_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         'C43 H35 Ir N4 O2, 2(C H Cl3)'
_chemical_formula_sum            'C45 H37 Cl6 Ir N4 O2'
_chemical_formula_weight         1070.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                82.0260(10)
_cell_angle_beta                 81.0530(10)
_cell_angle_gamma                78.2130(10)
_cell_formula_units_Z            2
_cell_length_a                   11.3980(7)
_cell_length_b                   12.2026(8)
_cell_length_c                   15.8397(10)
_cell_measurement_reflns_used    325
_cell_measurement_temperature    100
_cell_measurement_theta_max      45
_cell_measurement_theta_min      3
_cell_volume                     2117.3(2)
_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 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  0.0486
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23519
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        65.937
_diffrn_reflns_theta_max         65.937
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    9.938
_exptl_absorpt_correction_T_max  0.7513
_exptl_absorpt_correction_T_min  0.4826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_recrystallization_method CHCl3/Hexane
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.270
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.00010(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         7028
_refine_ls_number_restraints     420
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+7.1729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6901
_reflns_number_total             7028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00038_si_002.cif
_cod_data_source_block           dq24_0m
_cod_database_code               4089226
_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. Restrained distances
 Cl12-C4S = Cl11-C4S = Cl10-C4S
 1.76 with sigma of 0.02
 Cl7S-C3S = Cl9S-C3S = Cl8S-C3S
 1.76 with sigma of 0.02
 Cl3S-C1S = Cl1S-C1S = Cl2S-C1S
 1.76 with sigma of 0.02
 Cl5S-C2S = Cl4S-C2S = Cl6S-C2S
 1.76 with sigma of 0.02
 Cl3S-Cl1S
 2.88 with sigma of 0.04
 Cl1S-Cl2S
 2.88 with sigma of 0.04
 Cl3S-Cl2S
 2.88 with sigma of 0.04
 Cl4S-Cl5S
 2.88 with sigma of 0.04
 Cl6S-Cl4S
 2.88 with sigma of 0.04
 Cl6S-Cl5S
 2.88 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Sof(Cl5S)=Sof(Cl4S)=Sof(Cl6S)=Sof(C2S)=Sof(H2S)=1-FVAR(1)
 Sof(Cl3S)=Sof(Cl1S)=Sof(Cl2S)=Sof(C1S)=Sof(H1S)=FVAR(1)
 Sof(Cl10)=Sof(Cl12)=Sof(Cl11)=Sof(C4S)=Sof(H4S)=1-FVAR(2)
 Sof(Cl8S)=Sof(C3S)=Sof(H3S)=Sof(Cl7S)=Sof(Cl9S)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C4S(H4S), C1S(H1S), C2S(H2S), C3S(H3S)
5.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C41(H41), C20(H20), C19(H19), C26(H26), C25(H25), C14(H14),
 C13(H13), C5(H5), C22(H22), C32(H32), C10(H10), C42(H42), C28(H28), C3(H3),
 C27(H27), C31(H31), C2(H2), C33(H33), C15(H15), C21(H21), C4(H4), C8(H8)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C30(H30A,H30B,
 H30C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'