Unusual dual-emissive heteroleptic iridium complexes incorporating TADF cyclometalating ligands.
Benjamin, Helen; Zheng, Yonghao; Kozhevnikov, Valery N.; Siddle, Jamie S.; O'Driscoll, Luke J; Fox, Mark A.; Batsanov, Andrei S.; Griffiths, Gareth C.; Dias, Fernando B.; Monkman, Andrew P.; Bryce, Martin R.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2190–2208; doi:10.1039/c9dt04672k

data_7703413
_publ_section_title
;
 Unusual dual-emissive heteroleptic iridium complexes incorporating TADF
 cyclometalating ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2190
_journal_page_last               2208
_journal_paper_doi               10.1039/c9dt04672k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H34 F4 Ir N5 O2, 1.5(C6 H14)'
_chemical_formula_sum            'C53 H55 F4 Ir N5 O2'
_chemical_formula_weight         1062.22
_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   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-14
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972)
;
_audit_update_record
;
2019-11-14 deposited with the CCDC.	2020-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                60.9714(6)
_cell_angle_beta                 80.3094(7)
_cell_angle_gamma                68.9999(6)
_cell_formula_units_Z            2
_cell_length_a                   12.7257(3)
_cell_length_b                   14.9871(3)
_cell_length_c                   15.3105(3)
_cell_measurement_reflns_used    7131
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.30
_cell_volume                     2383.58(9)
_computing_cell_refinement       'SAINT version 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43033
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.006
_diffrn_reflns_theta_min         1.641
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2006/1 (Krause et al., 2015) was used for absorption correction. 
  R(int) was 0.0679 before and 0.0331 after correction. The Ratio 
  of minimum to maximum transmission is 0.6595. The \l/2 correction 
  factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1074
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.497
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         13912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0381P)^2^+0.0857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12254
_reflns_number_total             13912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04672k2.cif
_cod_data_source_block           2_09s337
_cod_depositor_comments
'Adding full bibliography for 7703413--7703414.cif.'
_cod_database_code               7703413
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Uiso(H20A)=Uiso(H20B)=Uiso(H20C)=FVAR(1)
 Uiso(H19A)=Uiso(H19B)=Uiso(H19C)=FVAR(2)
 Uiso(H18A)=Uiso(H18B)=Uiso(H18C)=FVAR(3)
 Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(4)
 Uiso(H39A)=Uiso(H39B)=Uiso(H39C)=FVAR(5)
 Uiso(H38A)=Uiso(H38B)=Uiso(H38C)=FVAR(6)
2.a Riding coordinates:
 C2(H2), C8(H8), C10(H10), C11(H11), C14(H14), C16(H16), C22(H22), C28(H28),
 C30(H30), C31(H31), C34(H34), C36(H36), C43(H43), C44(H44), C45(H45), C46(H46)
2.b Rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated (Rees et al., 2005) and 151 electrons were 
found in the volume of 705\%A^3^ in 1 void per unit cell. This is consistent 
with the presence of 1.5 molecules of hexane (C~6~H~14~) per Formula Unit, 
which account for 150 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              28895
_shelx_fab_checksum              88312
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'