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_7715176
_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, 1.54(C H2 Cl2)'
_chemical_formula_sum            'C43.54 H39.09 Cl3.09 F6 Ir N5 O4'
_chemical_formula_weight         1112.05
_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                 101.07(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.316(3)
_cell_length_b                   15.544(3)
_cell_length_c                   19.688(4)
_cell_measurement_reflns_used    62275
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.283
_cell_volume                     4599.9(16)
_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 0.984
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            62266
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.283
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.153
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.471333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1365 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.4713.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       block
_exptl_crystal_F_000             2203
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.950
_refine_diff_density_min         -1.772
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10403
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+12.1613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8712
_reflns_number_total             10403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03498d2.cif
_cod_data_source_block           sad_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7715174--7715176.cif.'
_cod_original_cell_volume        4600.0(17)
_cod_database_code               7715176
_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
 C42A-F1A
 1.3 with sigma of 0.02
 F2A-C42A
 1.3 with sigma of 0.02
 C42A-F3A
 1.3 with sigma of 0.02
 F1B-C42B
 1.3 with sigma of 0.02
 F2B-C42B
 1.3 with sigma of 0.02
 C42B-F3B
 1.3 with sigma of 0.02
 F2A-F1A
 2 with sigma of 0.02
 F1A-F3A
 2 with sigma of 0.02
 F2A-F3A
 2 with sigma of 0.02
 F1B-F3B
 2 with sigma of 0.02
 F2B-F1B
 2 with sigma of 0.02
 F2B-F3B
 2 with sigma of 0.02
 C42B-C5
 1.5 with sigma of 0.02
 C42A-C5
 1.5 with sigma of 0.02
3. Rigid bond restraints
 F3A, F2A, C42A, F1A, F1B, C42B, F3B, F2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl3, C44, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F5B, C40, F4B, F6B, F5A, F6A, F4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F3A \\sim F2A \\sim C42A \\sim F1A \\sim F1B \\sim C42B \\sim F3B \\sim F2B:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Cl3 \\sim C44 \\sim Cl4: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F5B \\sim C40 \\sim F4B \\sim F6B \\sim F5A \\sim F6A \\sim F4A: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F3B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F5B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F6B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(Cl3)=Sof(Cl4)=Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(1)
 Sof(Cl2)=Sof(Cl1)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(2)
 Sof(F3A)=Sof(F2A)=Sof(C42A)=Sof(F1A)=1-FVAR(3)
 Sof(F1B)=Sof(C42B)=Sof(F3B)=Sof(F2B)=FVAR(3)
 Sof(F5B)=Sof(F4B)=Sof(F6B)=1-FVAR(4)
 Sof(F5A)=Sof(F6A)=Sof(F4A)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B)
6.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C36(H36), C12(H12), C6(H6), C28(H28), C25(H25), C34(H34), C22(H22),
 C27(H27), C19(H19), C4(H4), C35(H35), C20(H20), C3(H3), C11(H11), C9(H9)
6.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C32(H32A,H32B,H32C), C16(H16A,H16B,
 H16C), C41(H41A,H41B,H41C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              66943
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'