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_4089224
_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         'C86 H76 Ir1 N6 O4, C H Cl3, C6 H14'
_chemical_formula_sum            'C93 H91 Cl3 Ir N6 O4'
_chemical_formula_weight         1847.46
_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             2017-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                82.055(3)
_cell_angle_beta                 71.844(2)
_cell_angle_gamma                84.427(3)
_cell_formula_units_Z            1
_cell_length_a                   11.0272(8)
_cell_length_b                   13.0954(9)
_cell_length_c                   15.9964(11)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.39
_cell_measurement_theta_min      3.41
_cell_volume                     2170.3(3)
_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 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0577
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23084
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        65.926
_diffrn_reflns_theta_max         65.926
_diffrn_reflns_theta_min         2.926
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.105
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.4019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1523 before and 0.0895 after correction. The Ratio of minimum to maximum transmission is 0.5339. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_recrystallization_method CHCl3/Hexane
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.147
_refine_diff_density_min         -2.731
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         7226
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0543
_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^)+(0.1036P)^2^+5.6459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6640
_reflns_number_total             7226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00038_si_002.cif
_cod_data_source_block           dq09_0m
_cod_original_formula_sum        'C93 H91 Cl3 Ir1 N6 O4'
_cod_database_code               4089224
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C17, Ir1, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C17 \\sim Ir1 \\sim O1: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) H32C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) Cl1(0.5) Cl3(0.5)
 Cl2(0.5) C48(0.5) H48A(0.5) H48B(0.5) C47(0.5) H47A(0.5) H47B(0.5) C46(0.5)
 H46A(0.5) H46B(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C33A(0.5) H33D(0.5)
 H33E(0.5) H33F(0.5) C32A(0.5) H32D(0.5) H32E(0.5) H32F(0.5) C34A(0.5)
 H34D(0.5) H34E(0.5) H34F(0.5) C44(0.5) H44(0.5) C45(0.5) H45A(0.5) H45B(0.5)
 H45C(0.5) C49(0.5) H49A(0.5) H49B(0.5)
5.a Ternary CH refined with riding coordinates:
 C44(H44)
5.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C47(H47A,H47B), C46(H46A,H46B), C49(H49A,H49B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C8(H8), C5(H5), C22(H22), C40(H40), C25(H25), C19(H19), C29(H29),
 C42(H42), C2(H2), C14(H14), C3(H3), C28(H28), C4(H4), C41(H41), C15(H15),
 C21(H21), C13(H13), C26(H26), C43(H43)
5.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C30(H30A,H30B,H30C), C33(H33A,H33B,
 H33C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C50(H50A,H50B,H50C),
 C33A(H33D,H33E,H33F), C32A(H32D,H32E,H32F), C34A(H34D,H34E,H34F), C45(H45A,
 H45B,H45C)
;
_shelx_res_checksum              83535
_shelx_hkl_checksum              82821
_olex2_submission_special_instructions 'No special instructions were received'