Multi-colour circularly polarized luminescence properties of chiral Schiff-base boron difluoride complexes
Ikeshita, Masahiro; Suzuki, Takato; Matsudaira, Kana; Kitahara, Maho; Imai, Yoshitane; Tsuno, Takashi; Physical Chemistry Chemical Physics  (2022) –; doi:10.1039/D2CP01861F

data_7245067
_publ_section_title
;
 Multi-colour circularly polarized luminescence properties of chiral
 Schiff-base boron difluoride complexes
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D2CP01861F
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H16 B F2 N O'
_chemical_formula_sum            'C19 H16 B F2 N O'
_chemical_formula_weight         323.14
_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     dual
_audit_creation_date             2022-02-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.334(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7506(8)
_cell_length_b                   6.4046(6)
_cell_length_c                   14.9030(14)
_cell_measurement_reflns_used    2571
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      26.2380
_cell_measurement_theta_min      2.3590
_cell_volume                     818.94(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Rigaku HyPix-3000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_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    -74.00 107.00   0.50    8.48    --   20.00  54.00 -30.00  362
  2  \w    -72.00  67.00   0.50    8.48    --   20.00  54.00-180.00  278
  3  \w     75.00 109.00   0.50    8.48    --   20.00  54.00-180.00   68
  4  \w    -70.00  -4.00   0.50    8.48    --   20.00  54.00 -60.00  132
  5  \w     15.00  53.00   0.50    8.48    --   20.00  54.00 -60.00   76
  6  \w     76.00 108.00   0.50    8.48    --   20.00  54.00 -60.00   64
  7  \w    -70.00 -15.00   0.50    8.48    --   20.00  54.00 -90.00  110
  8  \w     -3.00  58.00   0.50    8.48    --   20.00  54.00 -90.00  122
  9  \w     67.00 109.00   0.50    8.48    --   20.00  54.00 -90.00   84
 10  \w    -68.00 -43.00   0.50    8.48    --   20.00  54.00  60.00   50
 11  \w     23.00  99.00   0.50    8.48    --   20.00  54.00  60.00  152
 12  \w     -4.00  51.00   0.50    8.48    --   20.00  54.00-150.00  110
 13  \w     85.00 110.00   0.50    8.48    --   20.00  54.00-150.00   50
 14  \w    -49.00 -24.00   0.50    8.48    --   20.00  54.00   0.00   50
 15  \w     46.00  71.00   0.50    8.48    --   20.00  54.00   0.00   50
 16  \w    -68.00 109.50   0.50    8.48    --   20.00  54.00-120.00  355
;
_diffrn_measurement_device       'fixed-chi diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0328013000
_diffrn_orient_matrix_UB_12      -0.0026989000
_diffrn_orient_matrix_UB_13      0.0474716000
_diffrn_orient_matrix_UB_21      0.0756472000
_diffrn_orient_matrix_UB_22      0.0104961000
_diffrn_orient_matrix_UB_23      -0.0099797000
_diffrn_orient_matrix_UB_31      -0.0063455000
_diffrn_orient_matrix_UB_32      0.1101490000
_diffrn_orient_matrix_UB_33      0.0020922000
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15183
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.443
_diffrn_reflns_theta_min         2.374
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             336
_exptl_crystal_preparation       CH2Cl2/EtOH
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 889 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4710
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0540P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                2632
_reflns_number_total             4710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp01861f2.cif
_cod_data_source_block           exp_429
_cod_database_code               7245067
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H16NOBF2
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.958
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C11(H11)
1.b Aromatic/amide H refined with riding coordinates:
 C007(H007), C00A(H00A), C00B(H00B), C00D(H00D), C00F(H00F), C00G(H00G),
 C00H(H00H), C18(H18), C14(H14), C15(H15), C16(H16), C17(H17)
1.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              232
_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 1.572
_oxdiff_exptl_absorpt_empirical_full_min 0.736