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_7712354
_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 H9 Br F2 N2 O2 Pt, C17 H11 Br N2 O2 Pt'
_chemical_formula_sum            'C34 H20 Br2 F2 N4 O4 Pt2'
_chemical_formula_weight         1136.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 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.r6408)
;
_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                   18.1002(6)
_cell_length_b                   7.8365(2)
_cell_length_c                   20.7171(5)
_cell_measurement_reflns_used    5787
_cell_measurement_temperature    150
_cell_measurement_theta_max      77.1840
_cell_measurement_theta_min      4.2740
_cell_volume                     2938.56(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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     73.00  99.00   0.50   10.28    --   46.37 152.00  97.00   52
  2  \w     94.00 178.00   0.50   17.57    --  108.56  13.00 109.00  168
  3  \w     87.00 114.00   0.50   17.57    --  108.56-152.00  54.00   54
  4  \w     49.00  83.00   0.50   17.57    --  108.56-152.00  54.00   68
  5  \w     50.00 108.00   0.50   17.57    --  108.56 -99.00 120.00  116
  6  \w     33.00  69.00   0.50   17.57    --  108.56 -19.00  90.00   72
  7  \w     37.00  68.00   0.50   17.57    --  108.56 -37.00 150.00   62
  8  \w    -26.00  58.00   0.50   10.28    --   46.37 -37.00 120.00  168
  9  \w     75.00 101.00   0.50   17.57    --  108.56 -99.00-120.00   52
 10  \w     37.00  69.00   0.50   17.57    --  108.56 -37.00-180.00   64
 11  \w     71.00 111.00   0.50   10.28    --   46.37 125.00-180.00   80
 12  \w    -61.00 -15.00   0.50   10.28    --  -46.37  37.00-180.00   92
 13  \w   -157.00-112.00   0.50   17.57    --  -84.50-118.00 122.00   90
;
_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      -0.0197267000
_diffrn_orient_matrix_UB_12      -0.0714251000
_diffrn_orient_matrix_UB_13      0.0311303000
_diffrn_orient_matrix_UB_21      -0.0822789000
_diffrn_orient_matrix_UB_22      0.0183094000
_diffrn_orient_matrix_UB_23      0.0145677000
_diffrn_orient_matrix_UB_31      -0.0092089000
_diffrn_orient_matrix_UB_32      -0.0100716000
_diffrn_orient_matrix_UB_33      -0.1934132000
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9769
_diffrn_reflns_point_group_measured_fraction_full 0.859
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         4.268
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.286
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.572
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    2.569
_exptl_crystal_description       needle
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.421
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.271
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         4618
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0869P)^2^+4.8600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.669
_reflns_Friedel_fraction_full    0.713
_reflns_Friedel_fraction_max     0.707
_reflns_number_gt                4380
_reflns_number_total             4618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00192j3.cif
_cod_data_source_block           cocrystal12
_cod_database_code               7712354
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C17H9F2N2O2PtBrCl
_chemical_oxdiff_usercomment     150K
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.065
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(2)
 0.47(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
C16 \\sim N2 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C17: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
F2 \\sim C5 \\sim C4 \\sim C3 \\sim F1: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(C13) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C16, N2, C12, C13, C14, C15, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2, C5, C4, C3, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C20(H20), C2(H2), C8(H8), C25(H25), C14(H14), C21(H21), C26(H26),
 C19(H19), C28(H28), C27(H27), C29(H29), C9(H9), C32(H32), C11(H11), C31(H31),
 C4(H4), C15(H15), C10(H10), C22(H22)
;
_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 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.740