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_7714138
_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         'C60 H46 Cl2 Ir N5 O4'
_chemical_formula_sum            'C60 H46 Cl2 Ir N5 O4'
_chemical_formula_weight         1164.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                80.087(3)
_cell_angle_beta                 89.178(3)
_cell_angle_gamma                69.118(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8762(11)
_cell_length_b                   12.9389(11)
_cell_length_c                   15.9754(15)
_cell_measurement_reflns_used    9360
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      2.19
_cell_volume                     2446.4(4)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39476
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.381
_diffrn_reflns_theta_min         1.928
_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    2.894
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0809 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.8603.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       needle
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         9973
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0352P)^2^+3.3642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8412
_reflns_number_total             9973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02789a2.cif
_cod_data_source_block           me8
_cod_database_code               7714138
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.655
_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. Restrained distances
 N4-C27 \\sim N4-C0
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C61) = Uanis(C64) = Uanis(C63) = Uanis(C65) = Uanis(C62) = Uanis(C0) =
Uanis(C32) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31)
4. Others
 Fixed Sof: C61(0.5) H61(0.5) C64(0.5) H64(0.5) C63(0.5) H63(0.5) C65(0.5)
 H65(0.5) C62(0.5) H62(0.5) C0(0.5) C32(0.5) H32(0.5) C27(0.5) C28(0.5)
 H28(0.5) C29(0.5) H29(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C60(H60A,H60B), C58(H58A,H58B), C56(H56A,H56B), C59(H59A,H59B)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C22(H22), C21(H21), C5(H5), C36(H36), C16(H16), C17(H17), C2(H2),
 C3(H3), C24(H24), C48(H48), C45(H45), C18(H18), C43(H43), C42(H42), C9(H9),
 C44(H44), C13(H13), C37(H37), C51(H51), C52(H52), C54(H54), C10(H10), C34(H34),
  C12(H12), C35(H35), C61(H61), C64(H64), C63(H63), C65(H65), C62(H62),
 C11(H11), C55(H55), C32(H32), C28(H28), C29(H29), C30(H30), C31(H31)
5.c Fitted hexagon refined as free rotating group:
 C61(C64,C63,C65,C62,C0), C32(C27,C28,C29,C30,C31)
5.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_shelx_res_checksum              27633
_olex2_submission_special_instructions 'No special instructions were received'