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_4089225
_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         'C45 H36 Ir N3 O4, C1 H1 Cl3'
_chemical_formula_sum            'C46 H37 Cl3 Ir N3 O4'
_chemical_formula_weight         994.33
_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                83.390(5)
_cell_angle_beta                 87.362(5)
_cell_angle_gamma                69.548(4)
_cell_formula_units_Z            4
_cell_length_a                   12.121(3)
_cell_length_b                   13.114(3)
_cell_length_c                   26.530(6)
_cell_measurement_reflns_used    9811
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.82
_cell_measurement_theta_min      3.62
_cell_volume                     3924.9(16)
_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 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0512
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42318
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        66.161
_diffrn_reflns_theta_max         66.161
_diffrn_reflns_theta_min         1.676
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.869
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1333 before and 0.0911 after correction. The Ratio of minimum to maximum transmission is 0.5762. The \l/2 correction factor is 0.0015.'
_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    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_recrystallization_method CHCl3/Hex
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.183
_refine_diff_density_min         -5.200
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1020
_refine_ls_number_reflns         13071
_refine_ls_number_restraints     781
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1114P)^2^+34.1330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11960
_reflns_number_total             13071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00038_si_002.cif
_cod_data_source_block           dq04k_0m
_cod_original_cell_volume        3924.6(15)
_cod_database_code               4089225
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.618
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Cl12, Cl5S}
3. Restrained distances
 Cl2S-C1S = Cl3S-C1S = Cl1S-C1S
 1.78 with sigma of 0.02
 Cl3S-C1S = Cl2S-C1S = Cl1S-C1S
 1.78 with sigma of 0.02
 Cl8S-C3S = Cl7S-C3S = Cl3-C3S
 1.78 with sigma of 0.02
 Cl6S-C2S = Cl5S-C2S = Cl4S-C2S
 1.78 with sigma of 0.02
 Cl4S-C2S = Cl3A-C4S = Cl12-C4S = Cl5S-C2S = Cl11-C4S = Cl6S-C2S
 1.78 with sigma of 0.02
 Cl2S-Cl3S
 2.84 with sigma of 0.04
 Cl3S-Cl1S
 2.84 with sigma of 0.04
 Cl8S-Cl3
 2.84 with sigma of 0.04
 Cl7S-Cl3
 2.84 with sigma of 0.04
 Cl8S-Cl7S
 2.84 with sigma of 0.04
 Cl4S-Cl6S
 2.84 with sigma of 0.04
 Cl4S-Cl5S
 2.84 with sigma of 0.04
 Cl11-Cl12
 2.84 with sigma of 0.04
 Cl11-Cl3A
 2.84 with sigma of 0.04
 Cl12-Cl3A
 2.84 with sigma of 0.04
 Cl6S-Cl5S
 2.84 with sigma of 0.04
 Cl5S-Cl4S
 2.84 with sigma of 0.04
 Cl6S-Cl4S
 2.84 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(Cl6S) = Uanis(Cl11) = Uanis(C2S) = Uanis(C4S) = Uanis(Cl3A) = Uanis(Cl4S)
= Uanis(Cl12) = Uanis(Cl5S)
Uanis(C3S) = Uanis(Cl2S) = Uanis(Cl3) = Uanis(C1S) = Uanis(Cl8S) = Uanis(Cl1S)
= Uanis(Cl7S) = Uanis(Cl3S)
Uanis(Cl12) = Uanis(Cl5S)
5. Others
 Sof(Cl7S)=Sof(Cl3)=Sof(Cl8S)=Sof(C3S)=Sof(H3S)=1-FVAR(1)
 Sof(Cl1S)=Sof(Cl2S)=Sof(Cl3S)=Sof(C1S)=Sof(H1S)=FVAR(1)
 Sof(Cl5S)=Sof(Cl3A)=Sof(Cl11)=Sof(C4S)=Sof(H4S)=1-FVAR(2)
 Sof(Cl4S)=Sof(Cl6S)=Sof(C2S)=Sof(H2S)=Sof(Cl12)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S)
6.b Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N3(H3A,H3B)
6.c Aromatic/amide H refined with riding coordinates:
 C73(H73), C58(H58), C53(H53), C66(H66), C59(H59), C67(H67), C79(H79),
 C55(H55), C60(H60), C47(H47), C71(H71), C49(H49), C78(H78), C64(H64), C86(H86),
  C29(H29), C10(H10), C33(H33), C14(H14), C4(H4), C40(H40), C23(H23), C2(H2),
 C22(H22), C15(H15), C48(H48), C85(H85), C70(H70), C50(H50), C82(H82), C81(H81),
  C87(H87), C65(H65), C74(H74), C88(H88), C3(H3), C36(H36), C42(H42), C21(H21),
 C35(H35), C34(H34), C5(H5), C20(H20), C8(H8), C43(H43), C26(H26), C25(H25),
 C28(H28), C13(H13), C41(H41)
6.d Idealised Me refined as rotating group:
 C90(H90A,H90B,H90C), C38(H38A,H38B,H38C), C45(H45A,H45B,H45C), C75(H75A,H75B,
 H75C), C83(H83A,H83B,H83C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              17325
_shelx_hkl_checksum              46318
_olex2_submission_special_instructions 'No special instructions were received'