New phosphorescent iridium(III) dipyrrinato complexes: synthesis, emission properties and their deep red to near-infrared OLEDs.
Zhang, Hongyang; Wang, Haitao; Tanner, Kevin; Schlachter, Adrien; Chen, Zhao; Harvey, Pierre D.; Chen, Shuming; Wong, Wai-Yeung; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10629–10639; doi:10.1039/d1dt01557e

data_7707730
_publ_section_title
;
 New phosphorescent iridium(III) dipyrrinato complexes: synthesis,
 emission properties and their deep red to near-infrared OLEDs.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10629
_journal_page_last               10639
_journal_paper_doi               10.1039/d1dt01557e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C37 H27 Ir N4'
_chemical_formula_sum            'C37 H27 Ir N4'
_chemical_formula_weight         719.82
_chemical_name_systematic        Ir(ppy)2(dipyrrinato)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-15
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_audit_update_record
;
2020-05-23 deposited with the CCDC.	2021-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.834(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7181(15)
_cell_length_b                   9.2996(5)
_cell_length_c                   17.7227(16)
_cell_measurement_reflns_used    4211
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.3150
_cell_measurement_theta_min      2.5640
_cell_volume                     2863.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS 2018/3 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_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    -15.00  26.00   1.00    8.00    --  -11.59 -99.00-120.00   41
  2  \w      4.00  79.00   1.00    8.00    --   11.74  37.00  30.00   75
  3  \w    -54.00  53.00   1.00    8.00    --   11.74 -19.00  30.00  107
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0284471000
_diffrn_orient_matrix_UB_12      0.0124181000
_diffrn_orient_matrix_UB_13      -0.0167476000
_diffrn_orient_matrix_UB_21      0.0230185000
_diffrn_orient_matrix_UB_22      0.0360342000
_diffrn_orient_matrix_UB_23      0.0361407000
_diffrn_orient_matrix_UB_31      0.0180258000
_diffrn_orient_matrix_UB_32      -0.0660570000
_diffrn_orient_matrix_UB_33      0.0165832000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13690
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.312
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.696
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.062
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5034
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0581
_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^)+(0.0580P)^2^+14.3945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4060
_reflns_number_total             5034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01557e2.cif
_cod_data_source_block           xg0912
_cod_depositor_comments
'Adding full bibliography for 7707730--7707732.cif.'
_cod_database_code               7707730
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.626
_reflns_odcompleteness_completeness 99.94
_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. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C6)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C22(H22), C2(H2), C25(H25), C19(H19), C30(H30), C23(H23), C31(H31),
 C21(H21), C3(H3), C20(H20), C17(H17), C11(H11), C37(H37), C33(H33), C10(H10),
 C36(H36), C8(H8), C9(H9), C24(H24), C35(H35), C5(H5), C14(H14), C16(H16),
 C34(H34), C4(H4), C15(H15)
;
_shelx_res_checksum              11800
_shelx_hkl_checksum              79708
_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 1.465
_oxdiff_exptl_absorpt_empirical_full_min 0.780