Phosphorescent [3 + 2 + 1] coordinated Ir(iii) cyano complexes for achieving efficient phosphors and their application in OLED devices
Wu, Yuan; Yang, Chen; Liu, Jie; Zhang, Meng; Liu, Weiqiang; Li, Wansi; Wu, Chengcheng; Cheng, Gang; Yang, Qingdan; Wei, Guodan; Che, Chi-Ming; Chemical Science  (2021) –; doi:10.1039/D1SC01426A

data_1564022
_publ_section_title
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 Phosphorescent [3 + 2 + 1] coordinated Ir(iii) cyano complexes for
 achieving efficient phosphors and their application in OLED devices
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01426A
_journal_year                    2021
_chemical_formula_moiety         'C32 H31 F2 Ir N6 O, C2 H3 N'
_chemical_formula_sum            'C34 H34 F2 Ir N7 O'
_chemical_formula_weight         786.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
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_audit_update_record
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2021-03-11 deposited with the CCDC.	2021-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.01(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.448(10)
_cell_length_b                   19.35(2)
_cell_length_c                   19.23(2)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.826
_cell_measurement_theta_min      2.360
_cell_volume                     3131(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28353
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.812
_diffrn_reflns_theta_min         2.126
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.315
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1332 before and 0.0682 after correction.
The Ratio of minimum to maximum transmission is 0.7852.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_recrystallization_method MeCN/DCM/Et2O
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6663
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0001P)^2^+7.7911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4784
_reflns_number_total             6663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01426a2.cif
_cod_data_source_block           dfppy-OCN
_cod_original_cell_volume        3132(7)
_cod_database_code               1564022
_shelx_shelxl_version_number     2018/3
_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
N6 \\sim C32 \\sim O1: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
Uanis(N6) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(N6) = Uanis(C32)
3.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C13(H13A,H13B), C18(H18A,H18B), C14(H14A,H14B), C19(H19A,
 H19B), C15(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C22(H22), C2(H2), C3(H3), C28(H28), C8(H8), C11(H11), C31(H31),
 C7(H7), C6(H6), C24(H24), C29(H29), C30(H30)
3.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'