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_7245068
_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         'C23 H18 B F2 N O'
_chemical_formula_sum            'C23 H18 B F2 N O'
_chemical_formula_weight         373.19
_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             2021-12-09
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.7997(5)
_cell_length_b                   16.3983(8)
_cell_length_c                   22.9360(11)
_cell_measurement_reflns_used    6549
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      26.0520
_cell_measurement_theta_min      2.2330
_cell_volume                     3685.8(3)
_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 0.994
_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 -12.00   0.50    2.72    --   20.00  54.00 120.00  124
  2  \w     -6.00  20.00   0.50    2.72    --   20.00  54.00 120.00   52
  3  \w     36.00  62.00   0.50    2.72    --   20.00  54.00 120.00   52
  4  \w    -59.00 -31.00   0.50    2.72    --   20.00  54.00-150.00   56
  5  \w    -24.00  16.00   0.50    2.72    --   20.00  54.00-150.00   80
  6  \w    -70.00   8.00   0.50    2.72    --   20.00  54.00   0.00  156
  7  \w     39.00 100.00   0.50    2.72    --   20.00  54.00   0.00  122
  8  \w    -69.00  56.00   0.50    2.72    --   20.00  54.00 150.00  250
  9  \w    -74.00 -49.00   0.50    2.72    --   20.00  54.00  90.00   50
 10  \w     12.00  37.00   0.50    2.72    --   20.00  54.00  90.00   50
 11  \w    -67.00  29.00   0.50    2.72    --   20.00  54.00  60.00  192
;
_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      0.0057147000
_diffrn_orient_matrix_UB_12      0.0364121000
_diffrn_orient_matrix_UB_13      -0.0165144000
_diffrn_orient_matrix_UB_21      -0.0008098000
_diffrn_orient_matrix_UB_22      0.0232520000
_diffrn_orient_matrix_UB_23      0.0260709000
_diffrn_orient_matrix_UB_31      0.0721523000
_diffrn_orient_matrix_UB_32      -0.0026175000
_diffrn_orient_matrix_UB_33      0.0016236000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38018
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         30.356
_diffrn_reflns_theta_min         2.167
_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  0.92835
_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    1.345
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_preparation       CH2Cl2/EtOH
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.412
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 2445 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         10595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0900P)^2^+0.3980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                7277
_reflns_number_total             10595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp01861f2.cif
_cod_data_source_block           exp_438
_cod_database_code               7245068
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H18NOF2B
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C00J(H00J), C00L(H00L)
1.b Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00F(H00F), C00I(H00I), C00M(H00M), C00N(H00N), C00P(H00P),
 C00S(H00S), C00T(H00T), C00U(H00U), C00X(H00X), C00Y(H00Y), C010(H010),
 C011(H011), C012(H012), C013(H013), C014(H014), C015(H015), C016(H016),
 C018(H018), C019(H019), C01A(H01M), C01B(H01B), C01C(H01C), C01F(H01F),
 C01G(H01N), C01H(H01H), C01I(H01I), C01J(H01J)
1.c Idealised Me refined as rotating group:
 C017(H01G,H01K,H01L), C01D(H01A,H01D,H01E)
;
_shelx_res_checksum              98051
_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.907