Towards high performance solution-processed orange organic light-emitting devices: precisely-adjusting properties of Ir(iii) complexes by reasonably engineering the asymmetric configuration with second functionalized cyclometalating ligands
Sun, Yuanhui; Yang, Xiaolong; Liu, Boao; Dang, Jingshuang; Li, Yan; Zhou, Guijiang; Wu, Zhaoxin; Wong, Wai-Yeung; Journal of Materials Chemistry C 7 (2019) 8836–; doi:10.1039/C9TC02406A

data_7237863
_publ_section_title
;
 Towards high performance solution-processed orange organic light-emitting
 devices: precisely-adjusting properties of Ir(iii) complexes by
 reasonably engineering the asymmetric configuration with second
 functionalized cyclometalating ligands
;
_journal_issue                   29
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              8836
_journal_paper_doi               10.1039/C9TC02406A
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C51 H46 B Ir N2 O6 S2, 2(C H Cl3)'
_chemical_formula_sum            'C53 H48 B Cl6 Ir N2 O6 S2'
_chemical_formula_weight         1288.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-30 deposited with the CCDC.	2019-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                81.078(12)
_cell_angle_beta                 79.523(12)
_cell_angle_gamma                67.633(10)
_cell_formula_units_Z            2
_cell_length_a                   13.614(4)
_cell_length_b                   14.015(4)
_cell_length_c                   15.677(4)
_cell_measurement_reflns_used    9375
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4815
_cell_measurement_theta_min      1.3269
_cell_volume                     2707.9(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.533
_diffrn_reflns_theta_min         1.578
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.889
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       needle
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.269
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.607
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         12360
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0280P)^2^+9.3168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11715
_reflns_number_total             12360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9tc02406a3.cif
_cod_data_source_block           mx6208
_cod_original_cell_volume        2707.8(12)
_cod_database_code               7237863
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.510
_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
 Cl5A-C53 = Cl4-C53 = Cl4A-C53 = Cl6-C53 = Cl5-C53 = Cl6A-C53
 1.76 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl5) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(Cl6)
\\sim Ueq, Uanis(Cl5A) \\sim Ueq, Uanis(Cl6A) \\sim Ueq, Uanis(Cl4A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H53A)=Sof(Cl5A)=Sof(Cl6A)=Sof(Cl4A)=1-FVAR(1)
 Sof(Cl4)=Sof(Cl5)=Sof(Cl6)=Sof(H53)=FVAR(1)
5.a Riding coordinates:
 C18(H18A,H18B,H18C), C51(H51A,H51B,H51C)
5.b Ternary CH refined with riding coordinates:
 C52(H52), C53(H53), C53(H53A)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C14(H14), C16(H16),
 C23(H23), C25(H25), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C39(H39),
  C42(H42), C43(H43), C44(H44), C45(H45), C48(H48)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              1467
_olex2_submission_special_instructions 'No special instructions were received'