Tunability of triplet excited states and photophysical behaviour of bis-cyclometalated iridium(III) complexes with imidazo[4,5-<i>f</i>][1,10]phenanthroline.
Choroba, Katarzyna; Palion-Gazda, Joanna; Penkala, Mateusz; Rawicka, Patrycja; Machura, Barbara; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17934–17947; doi:10.1039/d4dt01996b

data_7717240
_publ_section_title
;
 Tunability of triplet excited states and photophysical behaviour of
 bis-cyclometalated iridium(III) complexes with
 imidazo[4,5-<i>f</i>][1,10]phenanthroline.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17934
_journal_page_last               17947
_journal_paper_doi               10.1039/d4dt01996b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C43 H28 Ir N6, F6 P'
_chemical_formula_sum            'C43 H28 F6 Ir N6 P'
_chemical_formula_weight         965.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-06-29
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-10 deposited with the CCDC.	2024-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2609(5)
_cell_length_b                   15.7886(5)
_cell_length_c                   15.9948(6)
_cell_measurement_reflns_used    9499
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7510
_cell_measurement_theta_min      3.7270
_cell_volume                     3853.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.879
_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    -39.00  14.00   1.00   69.52    --  -10.84  85.00 -94.00   53
  2  \w    -82.00  29.00   1.00   69.52    --  -10.84 -19.00  90.00  111
  3  \w     10.00  44.00   1.00   69.52    --  -10.84  38.00  60.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0371777000
_diffrn_orient_matrix_UB_12      -0.0256853000
_diffrn_orient_matrix_UB_13      0.0081049000
_diffrn_orient_matrix_UB_21      0.0179060000
_diffrn_orient_matrix_UB_22      0.0115154000
_diffrn_orient_matrix_UB_23      -0.0393063000
_diffrn_orient_matrix_UB_31      0.0213795000
_diffrn_orient_matrix_UB_32      0.0350207000
_diffrn_orient_matrix_UB_33      0.0188582000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21048
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.510
_diffrn_reflns_theta_min         3.627
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.987
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 2836 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0473P)^2^+1.0223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.745
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.801
_reflns_number_gt                7690
_reflns_number_total             9075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01996b2.cif
_cod_data_source_block           compound2
_cod_depositor_comments          'Adding full bibliography for 7717240.cif.'
_cod_database_code               7717240
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H26 N3 Ir1 P1 F6'
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.465
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C1(H1), C2(H2), C3(H3), C6(H6), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26),
  C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
 C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              71371
_shelx_hkl_checksum              30581
_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 1.506
_oxdiff_exptl_absorpt_empirical_full_min 0.792