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_7245070
_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         323.13
_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             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                 108.664(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3730(4)
_cell_length_b                   13.9191(4)
_cell_length_c                   11.5437(4)
_cell_measurement_reflns_used    8298
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.3140
_cell_measurement_theta_min      2.1420
_cell_volume                     1579.06(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.974
_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    -73.00 108.00   0.50    4.77    --   20.00  54.00  90.00  362
  2  \w    -73.00 -15.00   0.50    4.77    --   20.00  54.00 -30.00  116
  3  \w      3.00  33.00   0.50    4.77    --   20.00  54.00 -30.00   60
  4  \w    -71.00 -36.00   0.50    4.77    --   20.00  54.00-150.00   70
  5  \w    -17.00  60.00   0.50    4.77    --   20.00  54.00-150.00  154
  6  \w     73.00 110.00   0.50    4.77    --   20.00  54.00-150.00   74
  7  \w     -8.00  87.00   0.50    4.77    --   20.00  54.00 150.00  190
  8  \w    -52.00 -27.00   0.50    4.77    --   20.00  54.00-120.00   50
  9  \w    -20.00 110.00   0.50    4.77    --   20.00  54.00-120.00  260
 10  \w    -40.00 106.00   0.50    4.77    --   20.00  54.00   0.00  292
 11  \w    -45.00 -20.00   0.50    4.77    --   20.00  54.00 -60.00   50
 12  \w     -1.00  27.00   0.50    4.77    --   20.00  54.00 -60.00   56
 13  \w     68.00  94.00   0.50    4.77    --   20.00  54.00 -60.00   52
 14  \w    -69.00 -44.00   0.50    4.77    --   20.00  54.00  60.00   50
 15  \w     20.00  45.00   0.50    4.77    --   20.00  54.00  60.00   50
 16  \w    -32.00  -6.00   0.50    4.77    --   20.00  54.00-180.00   52
;
_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      -0.0236197000
_diffrn_orient_matrix_UB_12      0.0280162000
_diffrn_orient_matrix_UB_13      -0.0540292000
_diffrn_orient_matrix_UB_21      0.0252524000
_diffrn_orient_matrix_UB_22      -0.0349011000
_diffrn_orient_matrix_UB_23      -0.0319962000
_diffrn_orient_matrix_UB_31      -0.0633695000
_diffrn_orient_matrix_UB_32      -0.0243380000
_diffrn_orient_matrix_UB_33      -0.0163202000
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27219
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         30.499
_diffrn_reflns_theta_min         2.072
_diffrn_source                   'Sealed X-ray tube'
_diffrn_source_type              'Sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96113
_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    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_preparation       CH2Cl2/EtOH
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.305
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 2214 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9216
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                6157
_reflns_number_total             9216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cp01861f2.cif
_cod_data_source_block           exp_443
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C38 H32 B2 F4 N2 O2'
_cod_original_formula_weight         646.27
_cod_original_formula_moiety         '2(C19 H16 B F2 N O)'
_cod_original_formula_units_Z            2
_cod_database_code               7245070
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H16NOF2B
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C00E(H00E), C00R(H00R)
1.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00D(H00D), C00K(H00K), C00M(H00M), C00O(H00O), C00P(H00P),
 C00Q(H00Q), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C010(H010), C011(H011), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018), C01C(H01D)
1.c Idealised Me refined as rotating group:
 C00Z(H00A,H00B,H00C), C019(H01A,H01B,H01C)
;
_shelx_res_checksum              77263
_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 1.057
_oxdiff_exptl_absorpt_empirical_full_min 0.946