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_7703414
_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         'C48 H34 F4 Ir N5 O2, 4(C Cl3 D)'
_chemical_formula_sum            'C52 H34 Cl12 D4 F4 Ir N5 O2'
_chemical_formula_weight         1462.50
_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   mixed
_atom_sites_solution_primary     dual
_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                89.3872(15)
_cell_angle_beta                 76.7980(14)
_cell_angle_gamma                89.1792(15)
_cell_formula_units_Z            2
_cell_length_a                   10.0759(5)
_cell_length_b                   16.3073(8)
_cell_length_c                   17.9412(8)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.639
_cell_measurement_theta_min      2.410
_cell_volume                     2869.6(2)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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 multi-CPU (Sheldrick, 2015a)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59027
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        28.500
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.076
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.943
_exptl_absorpt_correction_T_max  0.8948
_exptl_absorpt_correction_T_min  0.8070
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
wR2(int) was 0.0591 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9019.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: d-chloroform'
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.059
_refine_diff_density_max         2.192
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         15449
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0398P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12529
_reflns_number_total             15449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04672k2.cif
_cod_data_source_block           3_19s248
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7703413--7703414.cif.
;
_cod_database_code               7703414
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.765
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1A
3. Same fragment restrains
{C12B, C13B, C14B, C15B, C16B, C17B, C18B, C19B, C20B} sigma for 1-2: 0.02,
1-3: 0.04
as in
{C12A, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A}
4. Others
 Uiso(H40A)=Uiso(H40B)=Uiso(H40C)=FVAR(1)
 Uiso(H38A)=Uiso(H38B)=Uiso(H38C)=FVAR(2)
 Sof(C12A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19A)=Sof(H19D)=
 Sof(H19E)=Sof(H19F)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(3)
 Sof(C12B)=Sof(C13B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(C16B)=Sof(H16B)=
 Sof(C17B)=Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19B)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(3)
 Fixed Sof: H39A(0.5) H39B(0.5) H39C(0.5) H39D(0.5) H39E(0.5) H39F(0.5)
5.a Riding coordinates:
 C18B(H18A,H18B,H18C), C19B(H19A,H19B,H19C), C20B(H20A,H20B,H20C), C18A(H18D,
 H18E,H18F), C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F)
5.b Ternary CH refined with riding coordinates:
 C50(D50), C51(D51), C49(D49), C52(D52)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C10(H10), C11(H11), C22(H22), C28(H28), C30(H30), C31(H31),
 C34(H34), C36(H36), C43(H43), C44(H44), C45(H45), C46(H46), C14B(H14B),
 C16B(H16B), C14A(H14A), C16A(H16A)
5.d Disordered Me refined with riding coordinates:
 C39(H39A,H39B,H39C,H39D,H39E,H39F)
5.e Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              8449
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'