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_4089228
_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         'C57 H44 Ir N2 O2 P, 0.5(C6 H14)'
_chemical_formula_sum            'C60 H51 Ir N2 O2 P'
_chemical_formula_weight         1055.20
_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                69.434(4)
_cell_angle_beta                 68.654(5)
_cell_angle_gamma                70.831(4)
_cell_formula_units_Z            4
_cell_length_a                   16.8060(14)
_cell_length_b                   16.8507(13)
_cell_length_c                   19.0323(16)
_cell_measurement_reflns_used    254
_cell_measurement_temperature    100
_cell_measurement_theta_max      3.54
_cell_measurement_theta_min      66.73
_cell_volume                     4574.2(7)
_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 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_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  0.0795
_diffrn_reflns_av_unetI/netI     0.0970
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30549
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        65.394
_diffrn_reflns_theta_max         65.394
_diffrn_reflns_theta_min         2.584
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    6.354
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.4624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.2463 before and 0.0911 after correction. The Ratio of minimum to maximum transmission is 0.6139. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.480
_refine_diff_density_min         -3.057
_refine_diff_density_rms         0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         14164
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0855
_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^)+(0.1233P)^2^+100.0004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2309
_refine_ls_wR_factor_ref         0.2449
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10742
_reflns_number_total             14164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00038_si_002.cif
_cod_data_source_block           dq19a_0m
_cod_database_code               4089228
_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. Uiso/Uaniso restraints and constraints
Uanis(C69) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C73) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C54) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C53) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C116(H11A,H11B), C117(H11C,H11D), C118(H11H,H11I), C119(H11J,H11K)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C61(H61), C50(H50), C47(H47), C3(H3), C59(H59), C53(H53), C62(H62),
 C15(H15), C4(H4), C13(H13), C51(H51), C57(H57), C49(H49), C60(H60), C8(H8),
 C54(H54), C48(H48), C14(H14), C5(H5), C2(H2), C55(H55), C72(H72), C41(H41),
 C109(H109), C97(H97), C65(H65), C100(H100), C84(H84), C98(H98), C76(H76),
 C20(H20), C70(H70), C94(H94), C79(H79), C77(H77), C107(H107), C111(H111),
 C99(H99), C37(H37), C105(H105), C71(H71), C39(H39), C85(H85), C38(H38),
 C101(H101), C19(H19), C83(H83), C104(H104), C114(H114), C45(H45), C106(H106),
 C21(H21), C67(H67), C30(H30), C56(H56), C108(H108), C22(H22), C113(H113),
 C44(H44), C81(H81), C42(H42), C112(H112), C78(H78), C25(H25), C95(H95),
 C27(H27), C26(H26), C96(H96), C43(H43)
3.c Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C29(H29A,H29B,
 H29C), C87(H87A,H87B,H87C), C115(H11E,H11F,H11G), C120(H12A,H12B,H12C),
 C90(H90A,H90B,H90C)
;
_shelx_res_checksum              21356
_shelx_hkl_checksum              6373
_olex2_submission_special_instructions 'No special instructions were received'