Elastic and bright assembly-induced luminescent crystal of platinum(II) complexes with near-unity emission quantum yield
Makino, Yusuke; Yoshida, Masaki; Hayashi, Shotaro; Sasaki, Toshiyuki; Takamizawa, Satoshi; Kobayashi, Atsushi; Kato, Masako; Dalton Transactions  (2023) –; doi:10.1039/D3DT00192J

data_7712353
_publ_section_title
;
 Elastic and bright assembly-induced luminescent crystal of platinum(II)
 complexes with near-unity emission quantum yield
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00192J
_journal_year                    2023
_chemical_formula_moiety         'C17 H11 Br N2 O2 Pt'
_chemical_formula_sum            'C17 H11 Br N2 O2 Pt'
_chemical_formula_weight         550.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-12-09 deposited with the CCDC.	2023-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.17880(10)
_cell_length_b                   20.8576(4)
_cell_length_c                   9.8686(2)
_cell_measurement_reflns_used    3922
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.6760
_cell_measurement_theta_min      4.2180
_cell_volume                     1477.65(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_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     18.00  68.00   0.50    7.54    --   46.37 -73.00 -23.00  100
  2  \w     69.00 102.00   0.50    5.66    --  108.56 -73.00 -23.00   66
  3  \w     36.00  64.00   0.50    5.66    --  108.56 -37.00 -60.00   56
  4  \w     35.00  75.00   0.50    5.66    --  108.56 -19.00 -30.00   80
  5  \w     44.00  75.00   0.50    5.66    --  108.56 -19.00  30.00   62
  6  \w     40.00  66.00   0.50    5.66    --  108.56 -37.00   0.00   52
  7  \w     35.00  66.00   0.50    5.66    --  108.56 -37.00 -30.00   62
  8  \w     36.00  64.00   0.50    5.66    --  108.56 -37.00 -90.00   56
  9  \w     40.00  66.00   0.50    5.66    --  108.56 -37.00-120.00   52
 10  \w     36.00  69.00   0.50    5.66    --  108.56 -37.00-180.00   66
 11  \w     36.00  66.00   0.50    5.66    --  108.56 -37.00-150.00   60
 12  \w    -24.00  15.00   0.50    7.54    --   46.37 -73.00 -23.00   78
 13  \w     35.00  60.00   0.50    5.66    --  108.56 -37.00 120.00   50
 14  \w     71.00 112.00   0.50    7.54    --   46.37 125.00  30.00   82
 15  \w     79.00 117.00   0.50    7.54    --   46.37 125.00 -30.00   76
 16  \w     72.00 103.00   0.50    7.54    --   46.37 125.00-180.00   62
 17  \w    -40.00 -15.00   0.50    5.66    --  -84.50  50.00 -42.00   50
 18  \w   -143.00-117.00   0.50    5.66    --  -84.50-112.00  93.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0582851000
_diffrn_orient_matrix_UB_12      0.1172378000
_diffrn_orient_matrix_UB_13      0.0445287000
_diffrn_orient_matrix_UB_21      0.1184764000
_diffrn_orient_matrix_UB_22      -0.0990136000
_diffrn_orient_matrix_UB_23      0.0399844000
_diffrn_orient_matrix_UB_31      0.1691048000
_diffrn_orient_matrix_UB_32      0.0289593000
_diffrn_orient_matrix_UB_33      -0.0432740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5744
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.736
_diffrn_reflns_theta_min         4.239
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.031
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45h (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_description       needle
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Flack x determined using 850 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.519
_reflns_Friedel_fraction_full    0.769
_reflns_Friedel_fraction_max     0.691
_reflns_number_gt                2541
_reflns_number_total             2670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00192j3.cif
_cod_data_source_block           2
_cod_database_code               7712353
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C17H11N2O2BrPt
_chemical_oxdiff_usercomment     150K
_shelx_estimated_absorpt_t_max   0.571
_shelx_estimated_absorpt_t_min   0.102
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C11(H11), C12(H12), C8(H8), C3(H3), C14(H14), C5(H5), C2(H2),
 C4(H4), C10(H10), C9(H9)
;
_shelx_res_checksum              74795
_shelx_hkl_checksum              98810
_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 1.707
_oxdiff_exptl_absorpt_empirical_full_min 0.627