Chiral iridium(iii) complexes with four-membered Ir-S-P-S chelating rings for high-performance circularly polarized OLEDs.
Yan, Zhi-Ping; Liao, Kang; Han, Hua-Bo; Su, Jian; Zheng, You-Xuan; Zuo, Jing-Lin; Chemical communications (Cambridge, England) 55 (2019) 8215–8218; doi:10.1039/c9cc03915e

data_7125375
_publ_section_title
;
 Chiral iridium(iii) complexes with four-membered Ir-S-P-S chelating rings
 for high-performance circularly polarized OLEDs.
;
_journal_issue                   57
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8215
_journal_page_last               8218
_journal_paper_doi               10.1039/c9cc03915e
_journal_volume                  55
_journal_year                    2019
_chemical_formula_moiety         'C50.04 H35.58 F6 Ir N4 O2 P S2'
_chemical_formula_sum            'C50.04 H35.42 F6 Ir N4 O2 P S2'
_chemical_formula_weight         1126.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-05-02 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.105(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0479(9)
_cell_length_b                   10.7246(11)
_cell_length_c                   25.204(3)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      53.98
_cell_measurement_theta_min      4.29
_cell_volume                     2421.2(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      192.98
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16720
_diffrn_reflns_point_group_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.984
_diffrn_reflns_theta_min         4.294
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.798
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4860
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       needle
_exptl_crystal_F_000             1115
_refine_diff_density_max         0.829
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.134(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         7820
_refine_ls_number_restraints     2456
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0513
_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^)+(0.0589P)^2^+3.2667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.689
_reflns_Friedel_fraction_full    0.772
_reflns_Friedel_fraction_max     0.763
_reflns_number_gt                7123
_reflns_number_total             7820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03915e2.cif
_cod_data_source_block           8HRP2
_cod_original_cell_volume        2421.3(4)
_cod_database_code               7125375
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.866(18)
 0.134(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C19-C24 = C24-C33 = C33-C47
 1.39 with sigma of 0.01
 C19-C33 = C24-C47
 2.37 with sigma of 0.02
 C2-C51 = C51-C39 = C25-C18 = C18-C2
 1.39 with sigma of 0.01
 C2-C39 = C39-C25 = C25-C2 = C18-C51
 2.37 with sigma of 0.02
 H9-H29
 2 with sigma of 0.01
 H30-H37
 2 with sigma of 0.01
4. Restrained planarity
 C19, C24, C33, C47
 with sigma of 0.02
 C2, C51, C39, C25, C18
 with sigma of 0.02
5. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3A with sigma of 0.01 and sigma
for terminal atoms of 0.02
7. 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
8. Others
 Fixed Sof: H25A(0.5) H25B(0.5) H2AA(0.5) H2AB(0.5) H4AA(0.5) H4AB(0.5)
9.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C25(H25A,H25B), C33(H33A,H33B), C39(H39A,H39B), C47(H47A,
 H47B), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB), C5AA(H5AA,H5AB), C4AA(H4AA,H4AB),
 C1AA(H1AA,H1AB), C6AA(H6AA,H6AB), C7AA(H7AA,H7AB)
9.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C21(H21), C22(H22), C23(H23),
 C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C37(H37), C38(H38),
  C45(H45), C48(H48), C50(H50), C0AA(H0AA)
;
_shelx_res_checksum              14905
_shelx_fab_checksum              96801
_olex2_submission_special_instructions 'No special instructions were received'