Circularly polarized phosphorescence with a large dissymmetry factor from a helical platinum(II) complex.
Ikeshita, Masahiro; Watanabe, Shinya; Suzuki, Seika; Tanaka, Shota; Hattori, Shingo; Shinozaki, Kazuteru; Imai, Yoshitane; Tsuno, Takashi; Chemical communications (Cambridge, England) 60 (2024) 2413–2416; doi:10.1039/d3cc06293g

data_7132652
_publ_section_title
;
 Circularly polarized phosphorescence with a large dissymmetry factor from
 a helical platinum(II) complex.
;
_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2413
_journal_page_last               2416
_journal_paper_doi               10.1039/d3cc06293g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C42 H30 N2 O Pt, C4 H8 O2'
_chemical_formula_sum            'C46 H38 N2 O3 Pt'
_chemical_formula_weight         861.87
_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     dual
_audit_creation_date             2023-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-12-21 deposited with the CCDC.	2024-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                77.263(4)
_cell_angle_beta                 82.321(3)
_cell_angle_gamma                84.958(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8643(3)
_cell_length_b                   11.6179(5)
_cell_length_c                   14.5758(8)
_cell_measurement_reflns_used    12008
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      26.9850
_cell_measurement_theta_min      1.9500
_cell_volume                     1775.15(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.937
_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     -7.00 109.00   0.50    7.34    --   20.00  54.00 -41.62  232
  2  \w    -74.00 -24.00   0.50    7.34    --   20.00  54.00 153.94  100
  3  \w    -10.00  15.00   0.50    7.34    --   20.00  54.00 153.94   50
  4  \w     57.00 105.00   0.50    7.34    --   20.00  54.00 153.94   96
  5  \w    -58.00 -32.00   0.50    7.34    --   20.00  54.00 -30.00   52
  6  \w     12.00 109.00   0.50    7.34    --   20.00  54.00 -30.00  194
  7  \w    -70.00 -26.00   0.50    7.34    --   20.00  54.00-120.00   88
  8  \w    -19.00  25.00   0.50    7.34    --   20.00  54.00-120.00   88
  9  \w     70.00  96.00   0.50    7.34    --   20.00  54.00-120.00   52
 10  \w     -7.00  39.00   0.50    7.34    --   20.00  54.00  60.00   92
 11  \w     46.00  78.00   0.50    7.34    --   20.00  54.00  60.00   64
 12  \w    -68.00 -43.00   0.50    7.34    --   20.00  54.00  30.00   50
 13  \w    -41.00 110.00   0.50    7.34    --   20.00  54.00  30.00  302
 14  \w    -74.00  93.00   0.50    7.34    --   20.00  54.00  90.00  334
 15  \w    -69.00 -42.00   0.50    7.34    --   20.00  54.00-150.00   54
 16  \w     45.00  72.00   0.50    7.34    --   20.00  54.00-150.00   54
 17  \w    -62.00  89.00   0.50    7.34    --   20.00  54.00 120.00  302
 18  \w    -73.00 -48.00   0.50    7.34    --   20.00  54.00-180.00   50
 19  \w    -70.00 -44.00   0.50    7.34    --   20.00  54.00   0.00   52
 20  \w    -73.00 -46.00   0.50    7.34    --   20.00  54.00 -41.62   54
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II (JP)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0071046000
_diffrn_orient_matrix_UB_12      -0.0010599000
_diffrn_orient_matrix_UB_13      0.0478561000
_diffrn_orient_matrix_UB_21      0.0651030000
_diffrn_orient_matrix_UB_22      0.0041365000
_diffrn_orient_matrix_UB_23      -0.0123446000
_diffrn_orient_matrix_UB_31      -0.0081828000
_diffrn_orient_matrix_UB_32      0.0625614000
_diffrn_orient_matrix_UB_33      -0.0090202000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0844
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36661
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         1.895
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_recrystallization_method EtOAc
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.146
_refine_diff_density_max         8.129
_refine_diff_density_min         -4.204
_refine_diff_density_rms         0.346
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         10206
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0722
_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^)+(0.1309P)^2^+2.0710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8651
_reflns_number_total             10206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06293g2.cif
_cod_data_source_block           exp_1053_auto
_cod_depositor_comments
'Adding full bibliography for 7132652--7132653.cif.'
_cod_original_cell_volume        1775.15(13)
_cod_database_code               7132652
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C42H30N2O1Pt1
_shelx_estimated_absorpt_t_max   0.593
_shelx_estimated_absorpt_t_min   0.428
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H51A,H51B,H51C} of C51, All C(H,H) groups
 At 1.5 times of:
  {H52A,H52B,H52C} of C52, {H23A,H23B,H23C} of C23
2. Rigid bond restraints
 C51, C50, O47, C48, O49
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C9, C11, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C51 \\sim C50 \\sim O47 \\sim C48 \\sim O49: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
C4 \\sim C9 \\sim C10 \\sim C11: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008 within 1.7A
4.a Ternary CH refined with riding coordinates:
 C22(H22)
4.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B)
4.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C20(H20), C14(H14), C44(H44), C11(H11), C13(H13), C38(H38),
 C19(H19), C33(H33), C36(H36), C42(H42), C45(H45), C30(H30), C34(H34), C43(H43),
  C35(H35), C7(H7), C10(H10), C8(H8), C18(H18), C16(H16), C29(H29), C17(H17),
 C26(H26), C27(H27), C28(H28)
4.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C52(H52A,H52B,H52C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              28515
_shelx_hkl_checksum              81454
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.813