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_4348461
_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 O8 S2, C H2 Cl2'
_chemical_formula_sum            'C33 H28 Cl2 F2 Ir N3 O8 S2'
_chemical_formula_weight         959.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-04-17
_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                 90.815(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1410(8)
_cell_length_b                   11.2575(9)
_cell_length_c                   29.700(3)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      2.27
_cell_volume                     3390.3(5)
_computing_cell_refinement       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.30C (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2008, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  D8Venture
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            31800
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.500
_diffrn_reflns_theta_min         2.270
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.287
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1077 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.7146.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.819
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8570
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0360P)^2^+4.9690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6489
_reflns_number_total             8570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            23.cif
_cod_data_source_block           23
_cod_database_code               4348461
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_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
 Cl2A-C2S \\sim Cl2-C1S \\sim Cl1-C1S \\sim Cl1A-C2S
 with sigma of 0.005
3. Others
 Fixed Sof: Cl1A(0.6) Cl2A(0.6) C2S(0.6) H2SA(0.6) H2SB(0.6) Cl1(0.4) Cl2(0.4)
 C1S(0.4) H1SA(0.4) H1SB(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C1S(H1SA,H1SB)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C19(H19), C25(H25), C26(H26), C27(H27),
 C28(H28), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17)
4.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C30(H30A,H30B,
 H30C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'