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_4348462
_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         'C52 H52 Ir N3 O10 S2, 4(C H2 Cl2)'
_chemical_formula_sum            'C56 H60 Cl8 Ir N3 O10 S2'
_chemical_formula_weight         1474.99
_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   geom
_atom_sites_solution_primary     heavy
_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                92.497(3)
_cell_angle_beta                 106.093(2)
_cell_angle_gamma                117.601(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6522(9)
_cell_length_b                   15.5667(10)
_cell_length_c                   15.8059(10)
_cell_measurement_reflns_used    9415
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      2.65
_cell_volume                     3006.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v.2013.4_1 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (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, 2015)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60242
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.154
_diffrn_reflns_theta_min         2.232
_diffrn_source                   'ImuS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.704
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1116 before and 0.0738 after correction.
The Ratio of minimum to maximum transmission is 0.5924.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.575
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.282
_refine_diff_density_max         5.435
_refine_diff_density_min         -2.444
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         17652
_refine_ls_number_restraints     674
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0680P)^2^+24.6750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15213
_reflns_number_total             17652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            31.cif
_cod_data_source_block           31
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4348462
_shelx_estimated_absorpt_t_max   0.516
_shelx_estimated_absorpt_t_min   0.305
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C38B-C37 \\sim C38A-C37
 with sigma of 0.02
 C38B-C39B \\sim C38A-C39A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl8A) = Uanis(Cl8B)
Uanis(Cl7A) = Uanis(Cl7B)
Uiso(C38B) = Uiso(C38A)
Uanis(C40B) = Uanis(C40A)
Uanis(C39A) = Uanis(C39B)
Uanis(C41A) = Uanis(C41B)
Uanis(C43B) = Uanis(C43A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H37(0.55) H37A(0.45) H42A(0.55) H42B(0.55) H42C(0.55) H42D(0.45)
 H42E(0.45) H42F(0.45) C38A(0.55) C39A(0.55) H39A(0.55) C40A(0.55) C41A(0.55)
 H41D(0.55) H41E(0.55) H41F(0.55) C43A(0.55) H43A(0.55) H43B(0.55) H43C(0.55)
 C38B(0.45) C39B(0.45) H39B(0.45) C40B(0.45) C41B(0.45) H41A(0.45) H41B(0.45)
 H41C(0.45) C43B(0.45) H43D(0.45) H43E(0.45) H43F(0.45) H56C(0.5) H56D(0.5)
 H56A(0.5) H56B(0.5) Cl7A(0.5) Cl8A(0.5) Cl7B(0.5) Cl8B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C55(H55A,H55B), C53(H53A,H53B), C56(H56C,H56D), C56(H56A,H56B)
6.b Me refined with riding coordinates:
 C42(H42A,H42B,H42C), C42(H42D,H42E,H42F)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C14(H14), C16(H16), C17(H17),
 C19(H19), C25(H25), C27(H27), C28(H28), C37(H37), C37(H37A), C46(H46),
 C48(H48), C39A(H39A), C39B(H39B)
6.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C41A(H41D,H41E,H41F), C43A(H43A,H43B,H43C),
 C41B(H41A,H41B,H41C), C43B(H43D,H43E,H43F)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'