Efficient yellow electroluminescence of four iridium(iii) complexes with benzo[d]thiazole derivatives as main ligands.
Niu, Zhi-Gang; Chen, Jun; Tan, Peng; Sun, Wei; Zheng, You-Xuan; Li, Gao-Nan; Zuo, Jing-Lin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8032–8040; doi:10.1039/c8dt01479e

data_7046425
_publ_section_title
;
 Efficient yellow electroluminescence of four iridium(iii) complexes with
 benzo[d]thiazole derivatives as main ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8032
_journal_page_last               8040
_journal_paper_doi               10.1039/c8dt01479e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C52 H34 F6 Ir N3 O2 P2 S2'
_chemical_formula_sum            'C52 H34 F6 Ir N3 O2 P2 S2'
_chemical_formula_weight         1165.08
_chemical_properties_physical    Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-11 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                109.056(2)
_cell_angle_beta                 109.8998(18)
_cell_angle_gamma                92.8019(18)
_cell_formula_units_Z            4
_cell_length_a                   14.2112(3)
_cell_length_b                   20.0703(5)
_cell_length_c                   20.8334(4)
_cell_measurement_reflns_used    14960
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5840
_cell_measurement_theta_min      2.1050
_cell_volume                     5194.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  82.00   1.00    6.00    --   11.53  77.00 -30.00  104
  2  \w    -68.00  23.00   1.00    6.00    --   11.53 -19.00-180.00   91
  3  \w     38.00  63.00   1.00    6.00    --   11.53  38.00 -60.00   25
  4  \w    -14.00  87.00   1.00    6.00    --   11.53  38.00 150.00  101
  5  \w    -14.00  36.00   1.00    6.00    --   11.53  57.00-120.00   50
  6  \w    -90.00 -57.00   1.00    6.00    --  -13.17-178.00 -60.00   33
  7  \w    -41.00 -16.00   1.00    6.00    --  -13.17 -57.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0120933000
_diffrn_orient_matrix_UB_12      0.0329544000
_diffrn_orient_matrix_UB_13      -0.0031529000
_diffrn_orient_matrix_UB_21      0.0292889000
_diffrn_orient_matrix_UB_22      0.0181553000
_diffrn_orient_matrix_UB_23      0.0379030000
_diffrn_orient_matrix_UB_31      0.0436790000
_diffrn_orient_matrix_UB_32      0.0054046000
_diffrn_orient_matrix_UB_33      -0.0081505000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54888
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.953
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1337
_refine_ls_number_reflns         21229
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0277P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15639
_reflns_number_total             21229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01479e2.cif
_cod_data_source_block           (cf3bt)2Ir(tpip)_sq
_cod_depositor_comments
'Adding full bibliography for 7046423--7046425.cif.'
_cod_database_code               7046425
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C104 H68 F12 Ir2 N6 O4 P4 S4'
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.732
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{C1, C1}
{C1, C1}
{C1, C1}
{C1, C1}
3. Restrained distances
 C86-C81
 1.43 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1_4) = Uanis(C1_3)
Uanis(C1_2) = Uanis(C1_1)
Uanis(C1_5) = Uanis(C1_6)
Uanis(C1_7) = Uanis(C1_8)
5. Same fragment restrains
{C1_3, F1_3, F2_3, F3_3}
{C1_4, F1_4, F2_4, F3_4}
{C1_5, F1_5, F2_5, F3_5}
{C1_7, F1_7, F2_7, F3_7}
{C1_8, F1_8, F2_8, F3_8}
as
{C1_1, F2_1, F1_1, F3_1} sigma for 1-2: 0.02 1-3: 0.04
6. Others
 Sof(C1)=Sof(F2)=Sof(F3)=Sof(F1)=1-FVAR(1)
 Sof(C1)=Sof(F2)=Sof(F1)=Sof(F3)=FVAR(1)
 Sof(C1)=Sof(F1)=Sof(F2)=Sof(F3)=1-FVAR(2)
 Sof(C1)=Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
 Sof(C1)=Sof(F4)=Sof(F5)=Sof(F6)=1-FVAR(3)
 Sof(C1)=Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
 Sof(C1)=Sof(F1)=Sof(F2)=Sof(F3)=1-FVAR(4)
 Sof(C1)=Sof(F1)=Sof(F2)=Sof(F3)=FVAR(4)
7.a Aromatic/amide H refined with riding coordinates:
 C57(H57), C56(H56), C11(H11), C26(H26), C78(H78), C71(H71), C24(H24), C2(H2),
 C16(H16), C63(H63), C62(H62), C5(H5), C61(H61), C54(H54), C10(H10), C19(H19),
 C23(H23), C25(H25), C92(H92), C36(H36), C18(H18), C100(H100), C4(H4), C12(H12),
  C9(H9), C101(H101), C82(H82), C40(H40), C46(H46), C64(H64), C75(H75),
 C94(H94), C88(H88), C104(H104), C70(H70), C91(H91), C90(H90), C77(H77),
 C76(H76), C68(H68), C95(H95), C42(H42), C102(H102), C89(H89), C98(H98),
 C39(H39), C84(H84), C45(H45), C38(H38), C96(H96), C37(H37), C30(H30),
 C103(H103), C86(H86), C52(H52), C34(H34), C48(H48), C43(H43), C83(H83),
 C97(H97), C44(H44), C50(H50), C51(H51), C85(H85), C33(H33), C32(H32), C49(H49),
  C31(H31)
;
_shelx_res_checksum              91805
_shelx_fab_checksum              35393
_platon_squeeze_void_probe_radius 1.20
_olex2_date_sample_data_collection 2016-05-05
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.360
_oxdiff_exptl_absorpt_empirical_full_min 0.838