Synthesis, characterization, and photoelectric properties of iridium(iii) complexes containing an N hetero-dibenzofuran C^N ligand
Ma, Zequn; Jing, Chaojun; Hang, Deyu; Fan, Hongtao; Duan, Lumeng; Fang, Shuqing; Yan, Li; RSC Advances 11 (2021) 11004–11010; doi:10.1039/D0RA10584H

data_7242417
_publ_section_title
;
 Synthesis, characterization, and photoelectric properties of iridium(iii)
 complexes containing an N hetero-dibenzofuran C^N ligand
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              11004
_journal_page_last               11010
_journal_paper_doi               10.1039/D0RA10584H
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C47 H36 Ir N4 O4, C6'
_chemical_formula_sum            'C53 H36 Ir N4 O4'
_chemical_formula_weight         985.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-19 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.067(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6837(5)
_cell_length_b                   14.4095(4)
_cell_length_c                   18.9429(5)
_cell_measurement_reflns_used    14867
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      73.3000
_cell_measurement_theta_min      3.9610
_cell_volume                     4726.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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    -93.00 -66.00   0.50    0.20    --  -46.95-134.00-163.00   54
  2  \w   -118.00 -64.00   0.50    0.20    --  -46.95-135.00  17.00  108
  3  \w    -98.00 -57.00   0.50    0.20    --  -46.95 135.00  83.00   82
  4  \w     41.00  99.00   0.50    0.20    --   46.95-135.00  17.00  116
  5  \w     53.00  79.00   0.50    0.20    --   46.95-134.00-163.00   52
  6  \w     71.00  99.00   0.50    0.20    --   46.95 135.00  83.00   56
  7  \w   -140.00-115.00   0.50    0.80    --  -99.00-135.00  17.00   50
  8  \w    -99.00 -74.00   0.50    0.80    --  -99.00 134.00 -96.00   50
  9  \w   -124.00 -56.00   0.50    0.80    --  -99.00 135.00  83.00  136
 10  \w     71.00  97.00   0.50    0.80    --  103.25-134.00-163.00   52
 11  \w     96.00 121.00   0.50    0.80    --  103.25 135.00  83.00   50
 12  \w     32.00 123.00   0.50    0.80    --  103.25-135.00  17.00  182
 13  \w     86.00 128.00   0.50    0.80    --  103.25 134.00 -96.00   84
 14  \w   -118.00 -75.00   0.50    0.20    --  -46.95-125.00-120.00   86
 15  \w   -118.00 -24.00   0.50    0.20    --  -46.95 -77.00  30.00  188
 16  \w     36.00 119.00   0.50    0.20    --   46.95  38.00-180.00  166
 17  \w   -111.00 -86.00   0.50    0.80    --  -99.00 -30.00 -90.00   50
 18  \w   -115.00 -83.00   0.50    0.80    --  -99.00  61.00 120.00   64
 19  \w     97.00 168.00   0.50    0.80    --  103.25  30.00 -90.00  142
 20  \w     32.00 126.00   0.50    0.80    --  103.25 -77.00   0.00  188
 21  \w     48.00  74.00   0.50    0.80    --  103.25 -94.00-180.00   52
 22  \w     91.00 168.00   0.50    0.80    --  103.25  45.00 -60.00  154
 23  \w     76.00 108.00   0.50    0.80    --  103.25 -94.00-180.00   64
 24  \w     33.00 115.00   0.50    0.80    --  103.25 -45.00 120.00  164
 25  \w     28.00 115.00   0.50    0.80    --  103.25 -30.00 -30.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0075612000
_diffrn_orient_matrix_UB_12      -0.0682443000
_diffrn_orient_matrix_UB_13      0.0649993000
_diffrn_orient_matrix_UB_21      -0.0067968000
_diffrn_orient_matrix_UB_22      -0.0823299000
_diffrn_orient_matrix_UB_23      -0.0540664000
_diffrn_orient_matrix_UB_31      0.0883906000
_diffrn_orient_matrix_UB_32      -0.0000743000
_diffrn_orient_matrix_UB_33      0.0235159000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41301
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.635
_diffrn_reflns_theta_min         2.552
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.997
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          2.194
_refine_ls_shift/su_mean         0.059
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+9.5504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6809
_reflns_number_total             9480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra10584h2.cif
_cod_data_source_block           tx1000
_cod_database_code               7242417
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNO
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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.a Ternary CH refined with riding coordinates:
 C38(H38)
2.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C26(H26), C12(H12), C25(H25), C29(H29), C21(H21), C30(H30),
 C13(H13), C20(H20), C1(H1), C4(H4), C19(H19), C18(H18), C3(H3), C2(H2),
 C36(H36), C41(H41), C44(H44), C39(H39)
2.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C17(H17A,H17B,H17C), C40(H40A,H40B,H40C), C47(H47A,H47B,
 H47C)
2.e :
 C45(H45)
;
_shelx_res_checksum              59400
_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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.771