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_7062718
_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, 1[CH3OH]'
_chemical_formula_sum            'C31 H21 F7 Ir N7 O'
_chemical_formula_weight         832.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2023-09-02
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-09-02 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.645(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.4391(11)
_cell_length_b                   16.4322(8)
_cell_length_c                   17.4014(7)
_cell_measurement_reflns_used    4319
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      73.5880
_cell_measurement_theta_min      3.3660
_cell_volume                     6079.6(5)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -33.00  64.00   1.00    1.43    --   40.73 -38.00  30.00   97
  2  \w     48.00  84.00   1.00    1.43    --   40.73-125.00  30.00   36
  3  \w     84.00 111.00   1.00    2.00    --  107.58 -77.00  30.00   27
  4  \w     69.00 102.00   1.00    2.00    --  107.58 -95.00  30.00   33
  5  \w     48.00 136.00   1.00    2.00    --  107.58 -30.00 150.00   88
  6  \w     32.00  59.00   1.00    2.00    --  107.58 -95.00  30.00   27
  7  \w     35.00  67.00   1.00    2.00    --  107.58 -77.00  30.00   32
  8  \w     33.00 108.00   1.00    2.00    --  107.58 -95.00 -90.00   75
  9  \w     48.00  80.00   1.00    1.43    --   40.73 -99.00-180.00   32
 10  \w     30.00 150.00   1.00    2.00    --  107.58 -15.00-120.00  120
 11  \w    145.00 172.00   1.00    2.00    --  107.58 125.00 -90.00   27
 12  \w    103.00 128.00   1.00    2.00    --  107.58 125.00  30.00   25
 13  \w   -110.00 -16.00   1.00    1.43    --  -40.73 -38.00-120.00   94
;
_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      0.0516374500
_diffrn_orient_matrix_UB_12      -0.0647732500
_diffrn_orient_matrix_UB_13      0.0319952000
_diffrn_orient_matrix_UB_21      0.0509848000
_diffrn_orient_matrix_UB_22      0.0663970000
_diffrn_orient_matrix_UB_23      0.0138788000
_diffrn_orient_matrix_UB_31      -0.0020560500
_diffrn_orient_matrix_UB_32      0.0131186500
_diffrn_orient_matrix_UB_33      0.0866572000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11590
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.399
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70429
_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    1.820
_exptl_crystal_description       needle
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.626
_refine_diff_density_min         -1.707
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         5379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0474P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4275
_reflns_number_total             5379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03513a2.cif
_cod_data_source_block           ir4-2
_cod_depositor_comments
'Adding full bibliography for 7062717--7062718.cif.'
_cod_database_code               7062718
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.525
_shelx_estimated_absorpt_t_min   0.358
_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), C26(H26), C27(H27), C28(H28), C29(H29)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 162 electrons were 
found in a volume of 976\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3OH] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93709
_shelx_fab_checksum              97331
_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 1.596
_oxdiff_exptl_absorpt_empirical_full_min 0.638