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_7132653
_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         'C30 H24 N2 O Pt'
_chemical_formula_sum            'C30 H24 N2 O Pt'
_chemical_formula_weight         623.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-03
_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                90
_cell_angle_beta                 98.051(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8288(4)
_cell_length_b                   15.4199(5)
_cell_length_c                   12.4090(4)
_cell_measurement_reflns_used    9533
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      29.7320
_cell_measurement_theta_min      2.1400
_cell_volume                     2241.08(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.951
_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     17.00  49.00   0.50    3.79    --   20.00  54.00 -90.00   64
  2  \w     62.00  90.00   0.50    3.79    --   20.00  54.00 -90.00   56
  3  \w    -74.00 109.00   0.50    3.79    --   20.00  54.00  30.00  366
  4  \w     16.00  41.00   0.50    3.79    --   20.00  54.00-150.00   50
  5  \w    -74.00 -23.00   0.50    3.79    --   20.00  54.00   0.00  102
  6  \w    -53.00  63.00   0.50    3.79    --   20.00  54.00 120.00  232
  7  \w     85.00 110.00   0.50    3.79    --   20.00  54.00 120.00   50
  8  \w    -74.00 -49.00   0.50    3.79    --   20.00  54.00 -30.00   50
  9  \w     10.00  35.00   0.50    3.79    --   20.00  54.00 -30.00   50
 10  \w     61.00 108.00   0.50    3.79    --   20.00  54.00 -30.00   94
 11  \w      6.00  31.00   0.50    3.79    --   20.00  54.00-180.00   50
 12  \w     37.00  62.00   0.50    3.79    --   20.00  54.00-120.00   50
 13  \w    -70.00 -45.00   0.50    3.79    --   20.00  54.00 -90.00   50
;
_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      -0.0468335000
_diffrn_orient_matrix_UB_12      -0.0057766000
_diffrn_orient_matrix_UB_13      0.0292835000
_diffrn_orient_matrix_UB_21      -0.0027394000
_diffrn_orient_matrix_UB_22      0.0454580000
_diffrn_orient_matrix_UB_23      0.0078015000
_diffrn_orient_matrix_UB_31      -0.0383400000
_diffrn_orient_matrix_UB_32      0.0038083000
_diffrn_orient_matrix_UB_33      -0.0491349000
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.566
_diffrn_reflns_theta_min         2.184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38036
_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    1.848
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method DMSO
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.194
_refine_diff_density_max         2.833
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0227P)^2^+3.6477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5361
_reflns_number_total             6539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06293g2.cif
_cod_data_source_block           exp_1084_auto
_cod_depositor_comments
'Adding full bibliography for 7132652--7132653.cif.'
_cod_database_code               7132653
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H24 N2 O1 Pt1'
_shelx_estimated_absorpt_t_max   0.375
_shelx_estimated_absorpt_t_min   0.179
_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 Ternary CH refined with riding coordinates:
 C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C28(H28), C3(H3), C4(H4), C32(H32), C27(H27), C6(H6), C33(H33),
 C18(H18), C8(H8), C31(H31), C34(H34), C16(H16), C24(H24), C25(H25), C22(H22),
 C14(H14), C23(H23), C17(H17), C15(H15)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_shelx_res_checksum              98400
_shelx_hkl_checksum              87716
_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 1.959
_oxdiff_exptl_absorpt_empirical_full_min 0.741