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_7245069
_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      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            4
_cell_length_a                   6.1678(14)
_cell_length_b                   8.1722(13)
_cell_length_c                   31.570(5)
_cell_measurement_reflns_used    1200
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      19.7160
_cell_measurement_theta_min      2.7840
_cell_volume                     1591.3(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.962
_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    -14.00  25.00   0.50   67.01    --   20.00  54.00 -30.00   78
  2  \w     28.00  54.00   0.50   67.01    --   20.00  54.00 -30.00   52
  3  \w     79.00 109.00   0.50   67.01    --   20.00  54.00 -30.00   60
  4  \w    -74.00  93.00   0.50   67.01    --   20.00  54.00 -90.00  334
  5  \w    -68.00 -43.00   0.50   67.01    --   20.00  54.00 -60.00   50
  6  \w    -22.00 110.00   0.50   67.01    --   20.00  54.00 -60.00  264
  7  \w     14.00  51.00   0.50   67.01    --   20.00  54.00-120.00   74
  8  \w     83.00 108.00   0.50   67.01    --   20.00  54.00-120.00   50
  9  \w    -67.00 -41.00   0.50   67.01    --   20.00  54.00   0.00   52
 10  \w    -71.00 -46.00   0.50   67.01    --   20.00  54.00 -30.00   50
;
_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      0.0084617000
_diffrn_orient_matrix_UB_12      0.0753078000
_diffrn_orient_matrix_UB_13      -0.0110756000
_diffrn_orient_matrix_UB_21      0.0044455000
_diffrn_orient_matrix_UB_22      -0.0430544000
_diffrn_orient_matrix_UB_23      -0.0194990000
_diffrn_orient_matrix_UB_31      -0.1144750000
_diffrn_orient_matrix_UB_32      0.0042410000
_diffrn_orient_matrix_UB_33      -0.0015501000
_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  0.1352
_diffrn_reflns_av_unetI/netI     0.2689
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            14957
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         30.543
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24387
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_preparation       CH2Cl2/EtOH
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 414 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.2598
_refine_ls_R_factor_gt           0.1104
_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^)+(0.0410P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.702
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                1834
_reflns_number_total             4620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp01861f2.cif
_cod_data_source_block           exp_459
_cod_database_code               7245069
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H16NOBF2
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.976
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Rigid bond restraints
 C009, C00C, C00G, N004, B1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
2. Uiso/Uaniso restraints and constraints
C009 \\sim C00C \\sim N004 \\sim B1 \\sim C00G: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002 within 1.7A
3.a Ternary CH refined with riding coordinates:
 C00C(H00C)
3.b Aromatic/amide H refined with riding coordinates:
 C005(H005), C007(H007), C00B(H00B), C00E(H00E), C00F(H00F), C00H(H00H),
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N)
3.c Idealised Me refined as rotating group:
 C00G(H00A,H00D,H00G)
;
_shelx_res_checksum              66808
_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 2.426
_oxdiff_exptl_absorpt_empirical_full_min 0.579