Highly phosphorescent iridium(iii) complexes based on 2-(biphenyl-4-yl)benzo[d]oxazole derivatives: synthesis, structures, properties and DFT calculations
Niu, Zhi-Gang; Zheng, Tao; Su, You-Hui; Wang, Peng-Jiang; Li, Xiao-Yan; Cui, Feng; Liang, Jiao; Li, Gao-Nan; New J. Chem. 39 (2015) 6025–; doi:10.1039/C5NJ00975H

data_7054883
_publ_section_title
;
 Highly phosphorescent iridium(iii) complexes based on
 2-(biphenyl-4-yl)benzo[d]oxazole derivatives: synthesis, structures,
 properties and DFT calculations
;
_journal_issue                   8
_journal_name_full               'New J. Chem.'
_journal_page_first              6025
_journal_paper_doi               10.1039/C5NJ00975H
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C43 H27 F4 Ir N2 O4, 0.5(C Cl4)'
_chemical_formula_sum            'C43.5 H27 Cl2 F4 Ir N2 O4'
_chemical_formula_weight         980.77
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-23 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.81340(16)
_cell_length_b                   14.81340(16)
_cell_length_c                   17.0733(4)
_cell_measurement_reflns_used    16132
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.9780
_cell_measurement_theta_min      2.7400
_cell_volume                     3746.51(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 10.5095
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -76.00  -32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       11.4559  178.0000  -90.0000 44

  2 omega  -75.00  -36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0184  132.0000 -147.6080 39

  3 omega -102.00   49.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0184    0.0000    0.0000 151

  4 omega  -81.00   17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0184  -57.0000  150.0000 98

  5 omega  -72.00    2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0184  127.0000  120.4353 74

  6 omega  -95.00   33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0184  -19.0000 -120.0000 128

  7 omega  -92.00  -67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.0184  157.0000  -40.1332 25
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0127203000
_diffrn_orient_matrix_UB_12      0.0305453000
_diffrn_orient_matrix_UB_13      0.0300206000
_diffrn_orient_matrix_UB_21      -0.0385244000
_diffrn_orient_matrix_UB_22      -0.0127810000
_diffrn_orient_matrix_UB_23      0.0220528000
_diffrn_orient_matrix_UB_31      0.0254856000
_diffrn_orient_matrix_UB_32      -0.0345687000
_diffrn_orient_matrix_UB_33      0.0183667000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45792
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.187
_diffrn_reflns_theta_max         25.187
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.855
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3369
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+18.4175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2471
_reflns_number_total             3369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00975h2.cif
_cod_data_source_block           wpj-8c
_cod_depositor_comments
;
Adding full bibliography for 7054880--7054883.cif.

2018-11-13
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C87 H54 Cl4 F8 Ir2 N4 O8'
_cod_original_formula_weight         1961.54
_cod_original_formula_moiety         '2(C43 H27 F4 Ir N2 O4), C Cl4'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        3746.50(11)
_cod_database_code               7054883
_chemical_oxdiff_formula         'C1 N1 O1 Ir1 F1'
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.550
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Cl1, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C2(H2), C9(H9), C12(H12), C19(H19), C5(H5), C15(H15), C3(H3),
 C4(H4), C17(H17), C21(H21)
4.b Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c)
;
_shelx_res_checksum              98074
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'