Rational design of efficient photosensitizers based on cyclometalated iridium(III) complexes with 2-arylbenzimidazole and aromatic 1,3-diketone ligands
Tatarin, Sergei V.; Meshcheriakova, Elizaveta A.; Kozyukhin, Sergey; Emets, Victor; Bezzubov, Stanislav; Dalton Transactions  (2023) –; doi:10.1039/D3DT02789A

data_7714144
_publ_section_title
;
 Rational design of efficient photosensitizers based on cyclometalated
 iridium(III) complexes with 2-arylbenzimidazole and aromatic 1,3-diketone
 ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02789A
_journal_year                    2023
_chemical_formula_moiety         'C76 H48 Cl2 F4 Ir2 N8, 4(C H Cl3)'
_chemical_formula_sum            'C80 H52 Cl14 F4 Ir2 N8'
_chemical_formula_weight         2081.99
_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     iterative
_audit_creation_date             2023-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-27 deposited with the CCDC.	2023-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.107(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4091(8)
_cell_length_b                   15.0372(5)
_cell_length_c                   25.0183(11)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      2.25
_cell_volume                     7581.2(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40903
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         1.949
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed X-ray tube'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.063
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_description       prism
_exptl_crystal_F_000             4064
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         9781
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0476P)^2^+65.8314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8037
_reflns_number_total             9781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02789a2.cif
_cod_data_source_block           vm3
_cod_database_code               7714144
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.497
_shelx_estimated_absorpt_t_min   0.356
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F1-C21
 1.35 with sigma of 0.02
 Cl06-C01H \\sim Cl1A-C01H
 with sigma of 0.02
 Cl2-C01H \\sim C01H-Cl06
 with sigma of 0.02
3. Restrained planarity
 C22, C21, C20, F1
 with sigma of 0.05
 F4, C1, C2, C3
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
Uiso(Cl2) = Uiso(Cl1A)
Uiso(F4) = Uiso(F1)
5. Others
 Fixed Sof: Cl1B(0.8) F3(0.8) H23(0.2) H21(0.8) F2(0.8) H2(0.8) H4(0.2)
 H01H(0.8) H01A(0.2) F4(0.2) F1(0.2) Cl1A(0.2) ClA(0.8) Cl2(0.2)
6.a Ternary CH refined with riding coordinates:
 C01H(H01H), C01H(H01A), C01I(H01I)
6.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C15(H15), C35(H35), C21(H21), C24(H24), C10(H10), C22(H22),
 C34(H34), C32(H32), C13(H13), C17(H17), C28(H28), C18(H18), C2(H2), C36(H36),
 C3(H3), C9(H9), C5(H5), C12(H12), C16(H16), C37(H37), C31(H31), C4(H4),
 C30(H30), C29(H29), C11(H11)
;
_shelx_res_checksum              92064
_olex2_submission_special_instructions 'No special instructions were received'