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_7125378
_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_absolute_configuration unk
_chemical_formula_moiety         'C50 H36 F6 Ir N4 O2 P S2'
_chemical_formula_sum            'C50 H36 F6 Ir N4 O2 P S2'
_chemical_formula_weight         1126.18
_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'
_symmetry_Int_Tables_number      4
_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                 97.7380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0612(5)
_cell_length_b                   10.7892(6)
_cell_length_c                   25.3691(14)
_cell_measurement_reflns_used    3699
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.49
_cell_volume                     2457.6(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9227
_diffrn_measured_fraction_theta_max 0.9227
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.1001
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16988
_diffrn_reflns_theta_full        24.9920
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    2.899
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.5218
_exptl_crystal_description       needle
_exptl_crystal_F_000             1114.6522
_refine_diff_density_max         0.8561
_refine_diff_density_min         -0.7094
_refine_diff_density_rms         0.1025
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.028(10)
_refine_ls_d_res_high            0.8411
_refine_ls_d_res_low             12.5690
_refine_ls_goodness_of_fit_ref   0.9963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    64
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7978
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      0.9910
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.0135
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.837
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              30
_reflns_limit_l_min              -30
_reflns_number_gt                6506
_reflns_number_total             7978
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9cc03915e2.cif
_cod_data_source_block           8HSP2
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7125378
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C50-C62
 1.45 with sigma of 0.02
 H17a-H26a
 2 with sigma of 0.01
 H34-H41
 2 with sigma of 0.01
 H33-H47
 2 with sigma of 0.01
3. Rigid bond restraints
 F1, F2, F3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C13, C70
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F4, C51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C50, C62
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C62
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C19, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F1, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F3, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C40, C42, C41, C70, C13, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C57, C49
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
F2 \\sim C56: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.001
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C46)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F3) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C17(H17a,H17b), C26(H26a,H26b), C45(H45a,H45b), C46(H46a,H46b), C48(H48a,
 H48b), C50(H50a,H50b), C62(H62a,H62b), C4(H4a,H4b)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C18(H18), C21(H21), C22(H22), C25(H25), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C41(H41), C47(H47), C49(H49),
  C57(H57), C59(H59), C70(H70), C5(H5), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'