Sulfonyl-Substituted Heteroleptic Cyclometalated Iridium(III) Complexes as Blue Emitters for Solution-Processable Phosphorescent Organic Light-Emitting Diodes.
Benjamin, Helen; Zheng, Yonghao; Batsanov, Andrei S.; Fox, Mark A.; Al-Attar, Hameed A; Monkman, Andrew P.; Bryce, Martin R.; Inorganic chemistry 55 (2016) 8612–8627; doi:10.1021/acs.inorgchem.6b01179

data_4348467
_publ_section_title
;
 Sulfonyl-Substituted Heteroleptic Cyclometalated Iridium(III) Complexes
 as Blue Emitters for Solution-Processable Phosphorescent Organic
 Light-Emitting Diodes.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8612
_journal_page_last               8627
_journal_paper_doi               10.1021/acs.inorgchem.6b01179
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C54 H37 F5 Ir N3 O7 S3, 2(C H2 Cl2), 0.85(C H4 O)'
_chemical_formula_sum            'C56.85 H44.4 Cl4 F5 Ir N3 O7.85 S3'
_chemical_formula_weight         1420.33
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5015(4)
_cell_length_b                   32.2402(12)
_cell_length_c                   14.4410(5)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.89
_cell_measurement_theta_min      2.29
_cell_volume                     5345.6(3)
_computing_cell_refinement       'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56931
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.263
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.893
_exptl_absorpt_correction_T_max  0.9385
_exptl_absorpt_correction_T_min  0.6421
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2010) was used for absorption correction.
wR2(int) was 0.0706 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.6842.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       needle
_exptl_crystal_F_000             2829
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     741
_refine_ls_number_reflns         9411
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0540P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7115
_reflns_number_total             9411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            15.cif
_cod_data_source_block           15
_cod_original_formula_sum        'C56.85 H44.40 Cl4 F5 Ir N3 O7.85 S3'
_cod_database_code               4348467
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.498
_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, All O(H) groups
2. Restrained distances
 Cl3-C56B \\sim Cl4A-C56B
 with sigma of 0.02
 Cl4A-C56A \\sim Cl3-C56A \\sim Cl4B-C56A
 with sigma of 0.02
3. Others
 Fixed Sof: Cl4A(0.85) Cl4B(0.15) C56A(0.75) H56A(0.75) H56B(0.75) C56B(0.25)
 H56C(0.25) H56D(0.25) O8(0.85) H8A(0.85) C57(0.85) H57A(0.85) H57B(0.85)
 H57C(0.85)
4.a Riding coordinates:
 C56A(H56A,H56B), O8(H8A), C57(H57A,H57B,H57C)
4.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56B(H56C,H56D)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C19(H19), C20(H20),
 C21(H21), C22(H22), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
  C35(H35), C36(H36), C38(H38), C39(H39), C42(H42), C43(H43), C45(H45),
 C46(H46), C49(H49), C50(H50), C52(H52), C53(H53)
4.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C47(H47A,H47B,H47C), C54(H54A,H54B,H54C)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'