Rational Design of Axially Chiral Platinabinaphthalenes with Aggregation-Induced Emission for Red Circularly Polarized Phosphorescent Organic Light-Emitting Diodes.
Jiang, Zhiyong; Wang, Jun; Gao, Tingting; Ma, Jianping; Chen, Runfeng; Liu, Zhipeng; ACS applied materials & interfaces  (2020) –; doi:10.1021/acsami.9b20568

data_4517401
_publ_section_title
;
 Rational Design of Axially Chiral Platinabinaphthalenes with
 Aggregation-Induced Emission for Red Circularly Polarized Phosphorescent
 Organic Light-Emitting Diodes.
;
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_paper_doi               10.1021/acsami.9b20568
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H27 N O4 Pt S'
_chemical_formula_sum            'C34 H27 N O4 Pt S'
_chemical_formula_weight         740.72
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-23
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.510(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9613(7)
_cell_length_b                   10.7014(4)
_cell_length_c                   13.1802(6)
_cell_measurement_reflns_used    2632
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.5640
_cell_measurement_theta_min      3.6590
_cell_volume                     1676.39(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1281
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.7555
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     32.00  65.00   1.00    1.00    --   36.73 -77.00  30.00   33
  2  \w     19.00  45.00   1.00    1.00    --   36.73 -57.00-150.00   26
  3  \w      3.00  63.00   1.00    1.00    --   36.73 -77.00 120.00   60
  4  \w      2.00  29.00   1.00    1.00    --   36.73 -99.00  30.00   27
  5  \w    -31.00  -5.00   1.00    1.00    --   36.73 -77.00  30.00   26
  6  \w     14.00  61.00   1.00    1.00    --   36.73  37.00  90.00   47
  7  \w     66.00 105.00   1.00    1.00    --   36.73  37.00  90.00   39
  8  \w     10.00  96.00   1.00    1.00    --   36.73  77.00 -30.00   86
  9  \w     41.00  75.00   1.00    1.00    --   36.73 -99.00  30.00   34
 10  \w     21.00  46.00   1.00    1.00    --   36.73  77.00 -90.00   25
 11  \w     57.00 103.00   1.00    1.00    --   36.73  77.00 -90.00   46
 12  \w    127.00 176.00   1.00    1.00    --  108.00  50.00 150.00   49
 13  \w     60.00 131.00   1.00    1.00    --  108.00 -37.00 150.00   71
 14  \w     86.00 114.00   1.00    1.00    --  108.00-111.00 120.00   28
 15  \w     44.00 123.00   1.00    1.00    --  108.00 -50.00 -30.00   79
 16  \w     47.00  83.00   1.00    1.00    --  108.00-111.00 120.00   36
 17  \w     42.00 114.00   1.00    1.00    --  108.00-111.00 -60.00   72
 18  \w     73.00 130.00   1.00    1.00    --  108.00 -77.00 120.00   57
 19  \w     39.00 136.00   1.00    1.00    --  108.00 -12.00  30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0257213000
_diffrn_orient_matrix_UB_12      -0.1407091000
_diffrn_orient_matrix_UB_13      -0.0013236000
_diffrn_orient_matrix_UB_21      0.1245649000
_diffrn_orient_matrix_UB_22      -0.0300638000
_diffrn_orient_matrix_UB_23      0.0276657000
_diffrn_orient_matrix_UB_31      0.0249879000
_diffrn_orient_matrix_UB_32      0.0051656000
_diffrn_orient_matrix_UB_33      0.1243938000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6778
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         70.99
_diffrn_reflns_theta_min         5.52
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.446
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4669
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                3993
_reflns_number_total             4669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am9b20568_si_002.cif
_cod_data_source_block           R-BP1
_cod_original_cell_volume        1676.38(14)
_cod_database_code               4517401
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C34(H34A,H34B,H34C)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C15(H15), C16(H16), C17(H17),
 C18(H18), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32)
2.c Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.578
_oxdiff_exptl_absorpt_empirical_full_min 0.581