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_4348466
_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         'C32 H26 F2 Ir N3 O10 S4, C2 H3 N'
_chemical_formula_sum            'C34 H29 F2 Ir N4 O10 S4'
_chemical_formula_weight         1012.05
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.004(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6275(5)
_cell_length_b                   15.3636(5)
_cell_length_c                   18.6894(7)
_cell_measurement_reflns_used    9828
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.93
_cell_measurement_theta_min      2.23
_cell_volume                     3559.2(2)
_computing_cell_refinement       'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_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 multi-CPU version (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_unetI/netI     0.0522
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63865
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.001
_diffrn_reflns_theta_min         1.643
_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    4.062
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2010) was used for absorption correction.
wR2(int) was 0.0999 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.7129.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.675
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         10367
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0460P)^2^+7.7970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7937
_reflns_number_total             10367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            13.cif
_cod_data_source_block           13
_cod_database_code               4348466
_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. Restrained distances
 Ir-C7B \\sim Ir-C7A
 with sigma of 0.005
 Ir-N2B \\sim Ir-N2A
 with sigma of 0.005
 C34-C33B \\sim C34-C33A
 with sigma of 0.02
 N4A-C33A \\sim N4B-C33B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S2A) = Uanis(S2B)
Uanis(F2B) = Uanis(F1A)
Uanis(C14B) = Uanis(C14A)
Uanis(C15B) = Uanis(C15A)
Uanis(C16B) = Uanis(C16A)
Uanis(C17B) = Uanis(C17A)
Uiso(N2B) = Uiso(N2A)
Uanis(C13B) = Uanis(C13A)
Uanis(C12B) = Uanis(C12A)
Uiso(C7B) = Uiso(C7A)
Uanis(C8B) = Uanis(C8A)
Uanis(C9B) = Uanis(C9A)
Uanis(C10B) = Uanis(C10A)
Uanis(C11B) = Uanis(C11A)
Uanis(O6B) = Uanis(O6A)
Uanis(O5B) = Uanis(O5A)
Uanis(S1B) = Uanis(S1A)
Uanis(O4B) = Uanis(O4A)
Uanis(C31B) = Uanis(C29A)
Uiso(O3B) = Uiso(O3A)
Uanis(C32B) = Uanis(C30A)
Uanis(N4B) = Uanis(N4A)
Uiso(C33A) = Uiso(C33B)
4. Same fragment restrains
{S1A, S2A, F1A, O3A, O4A, O5A, O6A, N2A, C7A, C8A, C9A, C10A, C11A, C12A, C13A,
C14A, C15A, C16A, C17A, C29A, C30A} sigma for 1-2: 0.02, 1-3: 0.04
as
{S1B, S2B, F2B, O3B, O4B, O5B, O6B, N2B, C7B, C8B, C9B, C10B, C11B, C12B, C13B,
C14B, C15B, C16B, C17B, C31B, C32B}
5. Others
 Sof(S1B)=Sof(S2B)=Sof(F2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(N2B)=
 Sof(C7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(C10B)=Sof(C11B)=Sof(C12B)=Sof(C13B)=
 Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=Sof(C17B)=
 Sof(H17B)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32B)=Sof(H32D)=
 Sof(H32E)=Sof(H32F)=Sof(N4B)=Sof(C33B)=1-FVAR(1)
 Sof(S1A)=Sof(S2A)=Sof(F1A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(N2A)=
 Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(C12A)=Sof(C13A)=
 Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=
 Sof(H17A)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=Sof(N4A)=Sof(C33A)=FVAR(1)
6.a Riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C19(H19), C25(H25), C26(H26), C27(H27),
 C28(H28), C8A(H8A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C29A(H29A,
 H29B,H29C), C30A(H30A,H30B,H30C), C8B(H8B), C14B(H14B), C15B(H15B), C16B(H16B),
  C17B(H17B), C31B(H31D,H31E,H31F), C32B(H32D,H32E,H32F), C34(H34A,H34B,H34C)
6.b Rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'