Asymmetric [Ir(C1^N1)(C2^N2)(L^X)]-tris-heteroleptic iridium(iii) complexes enable deep blue phosphorescent emission
Gu, Li; Li, Shuaibing; Han, Huabo; Wang, Xinzhong; Zhou, Changjiang; Lu, Junjian; Zhou, Liang; Lu, Guangzhao; New Journal of Chemistry 47 (2023) 18603–18609; doi:10.1039/D3NJ03513A

data_7062717
_publ_section_title
;
 Asymmetric [Ir(C1^N1)(C2^N2)(L^X)]-tris-heteroleptic iridium(iii)
 complexes enable deep blue phosphorescent emission
;
_journal_issue                   40
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18603
_journal_page_last               18609
_journal_paper_doi               10.1039/D3NJ03513A
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C30 H17 F7 Ir N7'
_chemical_formula_sum            'C30 H17 F7 Ir N7'
_chemical_formula_weight         800.71
_chemical_properties_physical    Air-sensitive,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-11
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-02-20 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.784(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8449(6)
_cell_length_b                   10.4597(4)
_cell_length_c                   34.0306(13)
_cell_measurement_reflns_used    5986
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.9280
_cell_measurement_theta_min      2.5630
_cell_volume                     5611.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     36.00  62.00   1.00    6.00    --   11.90 178.00   0.00   26
  2  \w      1.00  78.00   1.00    6.00    --   11.90  57.00 -90.00   77
  3  \w    -21.00  80.00   1.00    6.00    --   11.90  77.00   0.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0381494500
_diffrn_orient_matrix_UB_12      -0.0025599500
_diffrn_orient_matrix_UB_13      0.0092290500
_diffrn_orient_matrix_UB_21      0.0229850000
_diffrn_orient_matrix_UB_22      0.0139026000
_diffrn_orient_matrix_UB_23      0.0184704000
_diffrn_orient_matrix_UB_31      -0.0063265000
_diffrn_orient_matrix_UB_32      0.0663479000
_diffrn_orient_matrix_UB_33      -0.0035262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            14992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.608
_diffrn_reflns_theta_min         2.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.884
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5261
_reflns_number_total             6628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03513a2.cif
_cod_data_source_block           ir3
_cod_depositor_comments
'Adding full bibliography for 7062717--7062718.cif.'
_cod_database_code               7062717
_shelx_shelxl_version_number     2017/1
_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
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C12(H12), C14(H14), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              4336
_olex2_date_sample_data_collection 2022-01-11
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.718
_oxdiff_exptl_absorpt_empirical_full_min 0.720