Study of a phosphorescent cationic iridium(III) complex displaying blue shift in crystals
Martínez-Vollbert, Emiliano; Philouze, Christian; Gautier-Luneau, Isabelle; Moreau, Yohann; Lanoë, Pierre-Henri; Loiseau, Frederique; Physical Chemistry Chemical Physics  (2021) –; doi:10.1039/D1CP03341G

data_7243742
_publ_section_title
;
 Study of a phosphorescent cationic iridium(III) complex displaying blue
 shift in crystals
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP03341G
_journal_year                    2021
_chemical_formula_moiety         'C48 H50 Ir N6 O4, F6 P, 3(C2 H4 Cl2)'
_chemical_formula_sum            'C54 H62 Cl6 F6 Ir N6 O4 P'
_chemical_formula_weight         1408.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2021-03-24 deposited with the CCDC.	2021-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.07(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.554(4)
_cell_length_b                   22.055(4)
_cell_length_c                   15.394(3)
_cell_measurement_reflns_used    41641
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.000
_cell_measurement_theta_min      2.809
_cell_volume                     5912(3)
_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 0.999
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41641
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.625
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.576016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0922 before and 0.0353 after correction.
The Ratio of minimum to maximum transmission is 0.5760.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       plate
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.163
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         8603
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.803
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+12.8958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7680
_reflns_number_total             8603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp03341g2.cif
_cod_data_source_block           sad
_cod_original_cell_volume        5911(2)
_cod_database_code               7243742
_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
 Cl1B-C25B
 1.7 with sigma of 0.02
 C26B-Cl2B
 1.7 with sigma of 0.02
 C25B-C26B
 1.5 with sigma of 0.02
 C25B-Cl2B
 2.6 with sigma of 0.02
 Cl1B-C26B
 2.6 with sigma of 0.02
 C27A-Cl3
 1.7 with sigma of 0.01
 C27A-C27A_$1
 1.6 with sigma of 0.01
 C27A-Cl3_$1
 2.6 with sigma of 0.01
 C27B-Cl3
 1.7 with sigma of 0.01
 C27B-C27B_$1
 1.6 with sigma of 0.01
 C27B-Cl3_$1
 2.6 with sigma of 0.01
 C27B-Cl3
 1.7 with sigma of 0.01
 C19-C19_$2
 1.38 with sigma of 0.005
 N3-C19
 1.45 with sigma of 0.005
 C19-C20
 1.45 with sigma of 0.005
3. Rigid bond restraints
 Cl1B, Cl2B, C26B, C25B, Cl1A, C25A, C26A, Cl2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27A, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P1, F1, F2A, F3A, F3B, F2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl3, C27A, C27B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl1B \\sim Cl2B \\sim C26B \\sim C25B \\sim Cl1A \\sim C25A \\sim C26A \\sim
Cl2A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Cl3 \\sim C27A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
P1 \\sim F1 \\sim F2A \\sim F3A \\sim F3B \\sim F2B: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Cl3 \\sim C27A \\sim C27B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
5. Others
 Sof(Cl2B)=Sof(Cl1B)=Sof(C25B)=Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26C)=
 Sof(H26D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26A)=
 Sof(H26B)=FVAR(1)
 Sof(F2A)=Sof(F3A)=1-FVAR(2)
 Sof(F3B)=Sof(F2B)=FVAR(2)
 Sof(C27B)=Sof(H27C)=Sof(H27D)=1-FVAR(3)
 Sof(C27A)=Sof(H27A)=Sof(H27B)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C25A(H25A,H25B), C26A(H26A,H26B), C25B(H25C,H25D), C26B(H26C,H26D), C27A(H27A,
 H27B), C27B(H27C,H27D)
6.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C23(H23), C12(H12), C9(H9), C5(H5), C2(H2), C22(H22), C10(H10),
 C4(H4)
6.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              25602
_shelx_hkl_checksum              73193
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'