Neutral 2-phenylbenzimidazole-based iridium(III) complexes with picolinate ancillary ligand: tuning the emission properties by manipulating the substituent on the benzimidazole ring.
Martínez-Vollbert, Emiliano; Philouze, Christian; Cavignac, Théo; Latouche, Camille; Loiseau, Frédérique; Lanoë, Pierre-Henri; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4705–4718; doi:10.1039/d3dt03498d

data_7715174
_publ_section_title
;
 Neutral 2-phenylbenzimidazole-based iridium(III) complexes with
 picolinate ancillary ligand: tuning the emission properties by
 manipulating the substituent on the benzimidazole ring.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4705
_journal_page_last               4718
_journal_paper_doi               10.1039/d3dt03498d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C42 H36 F6 Ir N5 O4'
_chemical_formula_sum            'C42 H36 F6 Ir N5 O4'
_chemical_formula_weight         980.96
_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     direct
_audit_creation_date             2023-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2023-03-06 deposited with the CCDC.	2023-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                85.63(3)
_cell_angle_beta                 88.84(3)
_cell_angle_gamma                78.87(3)
_cell_formula_units_Z            2
_cell_length_a                   11.392(2)
_cell_length_b                   11.878(2)
_cell_length_c                   14.728(3)
_cell_measurement_reflns_used    45506
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.000
_cell_measurement_theta_min      2.296
_cell_volume                     1949.7(7)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT-2016 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45506
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.296
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.502
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.576749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0600 before and 0.0325 after correction.
The Ratio of minimum to maximum transmission is 0.5767.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         11358
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+1.1400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0487
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10433
_reflns_number_total             11358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03498d2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7715174--7715176.cif.'
_cod_database_code               7715174
_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
2. Restrained distances
 O4A-C41A
 1.4 with sigma of 0.02
 O4B-C41B
 1.4 with sigma of 0.02
3. Rigid bond restraints
 C40, F1B, F2A, F3A, F3B, F1A, F2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C42, F4A, F5B, F6A, F5A, F4B, F6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4A, C21, C41A, O4A, C41A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4A, C21, C41A, O4B, C41B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C42 \\sim F4A \\sim F5B \\sim F6A \\sim F5A \\sim F4B \\sim F6B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C40 \\sim F1B \\sim F2A \\sim F3A \\sim F3B \\sim F1A \\sim F2B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
O4A \\sim C21 \\sim C41A \\sim O4A \\sim C41A: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
O4A \\sim C21 \\sim C41A \\sim O4B \\sim C41B: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(F5B) \\sim Ueq, Uanis(F4B) \\sim Ueq, Uanis(C41B) \\sim Ueq, Uanis(F5A)
\\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F3A) \\sim Ueq, Uanis(F1B) \\sim Ueq, Uanis(F6B) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.01
5. Others
 Sof(F5B)=Sof(F4B)=Sof(F6B)=1-FVAR(1)
 Sof(F4A)=Sof(F6A)=Sof(F5A)=FVAR(1)
 Sof(F1B)=Sof(F3B)=Sof(F2B)=1-FVAR(2)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=FVAR(2)
 Sof(O4A)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=1-FVAR(3)
 Sof(O4B)=Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C14(H14)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C28(H28), C22(H22), C34(H34), C12(H12), C37(H37), C4(H4),
 C36(H36), C25(H25), C19(H19), C26(H26), C20(H20), C35(H35), C9(H9), C10(H10)
6.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C31(H31A,H31B,H31C), C15(H15A,H15B,H15C), C32(H32A,H32B,
 H32C), C16(H16A,H16B,H16C), C41A(H41A,H41B,H41C), C41B(H41D,H41E,H41F)
;
_shelx_res_checksum              53451
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'