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_7715175
_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         'C40 H32 F6 Ir N5 O2, C H2 Cl2'
_chemical_formula_sum            'C41 H34 Cl2 F6 Ir N5 O2'
_chemical_formula_weight         1005.83
_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
_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                90
_cell_angle_beta                 102.83(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.113(3)
_cell_length_b                   15.027(3)
_cell_length_c                   17.152(3)
_cell_measurement_reflns_used    50004
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.388
_cell_volume                     4049.3(14)
_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 0.996
_diffrn_measured_fraction_theta_max 0.990
_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  0.0338
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50004
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.388
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.499
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.401689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0603 before and 0.0343 after correction.
The Ratio of minimum to maximum transmission is 0.4017.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.185
_refine_diff_density_min         -2.215
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9220
_refine_ls_number_restraints     185
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0247P)^2^+17.9483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7389
_reflns_number_total             9220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03498d2.cif
_cod_data_source_block           sad_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7715174--7715176.cif.'
_cod_original_cell_volume        4049.4(15)
_cod_database_code               7715175
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 F5B, C40, F6B, F4B, F4A, F6A, F5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C39, F2A, F3A, F1A, F2B, F3B, F1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C41, Cl1, Cl2A, Cl2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F5B \\sim C40 \\sim F6B \\sim F4B \\sim F4A \\sim F6A \\sim F5A: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C39 \\sim F2A \\sim F3A \\sim F1A \\sim F2B \\sim F3B \\sim F1B: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
C41 \\sim Cl1 \\sim Cl2A \\sim Cl2B: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(F1B) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H41C)=Sof(H41D)=Sof(Cl2B)=1-FVAR(1)
 Sof(Cl2A)=Sof(H41A)=Sof(H41B)=FVAR(1)
 Sof(F2B)=Sof(F3B)=Sof(F1B)=1-FVAR(2)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=FVAR(2)
 Sof(F4A)=Sof(F6A)=Sof(F5A)=1-FVAR(3)
 Sof(F5B)=Sof(F6B)=Sof(F4B)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C14(H14), C30(H30)
5.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C41(H41C,H41D)
5.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C37(H37), C6(H6), C22(H22), C28(H28), C35(H35), C36(H36), C3(H3),
 C27(H27), C4(H4), C20(H20), C19(H19), C12(H12), C25(H25), C9(H9), C11(H11),
 C26(H26), C10(H10)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C31(H31A,H31B,H31C), C15(H15A,H15B,H15C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              11866
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'