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_7714149
_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         'C100 H68 Cl2 Ir2 N8, 2.25(C0.8 H1.6 Cl1.6)'
_chemical_formula_sum            'C101.8 H71.6 Cl5.6 Ir2 N8'
_chemical_formula_weight         1989.79
_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                103.9670(10)
_cell_angle_beta                 93.2770(10)
_cell_angle_gamma                101.9530(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0955(3)
_cell_length_b                   19.1698(6)
_cell_length_c                   19.3990(5)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.38
_cell_measurement_theta_min      2.23
_cell_volume                     4593.9(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.977
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30399
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.831
_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    3.107
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0928 before and 0.0443 after correction.
The Ratio of minimum to maximum transmission is 0.6705.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             1975
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.868
_refine_diff_density_min         -1.588
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         17642
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0478P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13309
_reflns_number_total             17642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02789a2.cif
_cod_data_source_block           st224
_cod_original_formula_sum        'C101.80 H71.60 Cl5.60 Ir2 N8'
_cod_database_code               7714149
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.370
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Cl5-C03E
 1.75 with sigma of 0.005
 Cl07-C03E
 1.75 with sigma of 0.005
 Cl07-C03E \\sim Cl6-C03E \\sim Cl00-C03E \\sim Cl5-C03E
 with sigma of 0.01
 Cl3-C51 \\sim Cl3-C03K \\sim Cl06-C03K \\sim Cl06-C51
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl5) = Uanis(Cl00)
Uanis(Cl07) = Uanis(Cl6)
Uanis(Cl5) = Uanis(Cl00) = Uanis(C03E) = Uanis(Cl07) = Uanis(Cl6)
Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C14) = Uanis(C15)
4. Others
 Fixed Sof: Cl06(0.8) Cl07(0.6) Cl00(0.6) Cl3(0.8) H03C(0.6) H03D(0.6)
 H03E(0.4) H03F(0.4) C03K(0.6) H03I(0.6) H03J(0.6) Cl5(0.4) Cl6(0.4) C51(0.2)
 H51A(0.2) H51B(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C03E(H03C,H03D), C03E(H03E,H03F), C03K(H03I,H03J), C51(H51A,H51B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C00Z(H00Z), C010(H010), C49(H49), C24(H24), C01C(H01C), C27(H27),
 C01E(H01E), C11(H11), C01I(H01I), C19(H19), C01O(H01O), C01Q(H01Q), C01R(H01R),
  C46(H46), C01U(H01U), C36(H36), C48(H48), C01X(H01X), C01Y(H01Y), C10(H10),
 C21(H21), C021(H021), C023(H023), C40(H40), C23(H23), C22(H22), C027(H027),
 C43(H43), C35(H35), C9(H9), C47(H47), C02C(H02C), C02E(H02E), C02F(H02F),
 C42(H42), C02H(H02H), C02I(H02I), C02J(H02J), C02K(H02K), C44(H44), C02M(H02M),
  C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q), C02S(H02S), C17(H17),
 C02V(H02V), C5(H5), C15(H15), C02Z(H02Z), C41(H41), C30(H30), C18(H18), C8(H8),
  C34(H34), C6(H6), C7(H7), C31(H31), C038(H038), C32(H32), C03A(H03A),
 C03B(H03B), C33(H33), C16(H16), C03G(H03G), C03H(H03H)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64140
_shelx_fab_checksum              12582
_olex2_submission_special_instructions 'No special instructions were received'