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_7714148
_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         'C80 H60 Cl2 Ir2 N8 O4, C H4 O'
_chemical_formula_sum            'C81 H64 Cl2 Ir2 N8 O5'
_chemical_formula_weight         1684.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 108.1450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4452(6)
_cell_length_b                   15.2416(4)
_cell_length_c                   23.5774(7)
_cell_measurement_reflns_used    9794
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.49
_cell_measurement_theta_min      2.24
_cell_volume                     6981.8(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.616
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_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    3.944
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.4418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1465 before and 0.0647 after correction. The Ratio of minimum to maximum transmission is 0.5921. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       block
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.804
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         12349
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0474P)^2^+20.4334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9915
_reflns_number_total             12349
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02789a2.cif
_cod_data_source_block           vm2
_cod_database_code               7714148
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.506
_shelx_estimated_absorpt_t_min   0.451
_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, All O(H) groups
2. Restrained distances
 O3-C42
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C42) = Uanis(O3)
4. Others
 Fixed Sof: O1(0.5) H1(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) O3(0.5)
 H3A(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C00T(H00T), C16(H16), C14(H14), C013(H013), C6(H6),
 C2(H2), C18(H18), C17(H17), C3(H3), C01C(H01C), C30(H30), C39(H39), C23(H23),
 C01H(H01H), C10(H10), C01J(H01J), C01K(H01K), C26(H26), C01P(H01P), C01Q(H01Q),
  C34(H34), C01T(H01T), C01U(H01U), C13(H13), C36(H36), C01X(H01X), C11(H11),
 C021(H021), C31(H31), C32(H32), C38(H38), C33(H33), C027(H027), C028(H028),
 C12(H12), C37(H37), C02C(H02C), C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G),
  C02H(H02H), C02J(H02J), C02K(H02K), C02L(H02L), C02M(H02M)
5.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C5(H5A,H5B,H5C), C02N(H02A,H02B,H02I), C02P(H02N,H02O,
 H02P), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3A)
;
_shelx_res_checksum              7472
_olex2_submission_special_instructions 'No special instructions were received'