Blue fluorescence from N,O-coordinated BF2 complexes having aromatic chromophores in solution and solid state
Yamaji, Minoru; Tomonari, Kazuhiro; Ikuma, Keisuke; Goto, Kenta; Tani, Fumito; Okamoto, Hideki; Photochemical & Photobiological Sciences  (2019) –; doi:10.1039/C9PP00410F

data_1552887
_publ_section_title
;
 Blue fluorescence from N,O-coordinated BF2 complexes having aromatic
 chromophores in solution and solid state
;
_journal_name_full               'Photochemical &amp; Photobiological Sciences'
_journal_paper_doi               10.1039/C9PP00410F
_journal_year                    2019
_chemical_formula_moiety         'C20 H13 B F2 N2 O'
_chemical_formula_sum            'C20 H13 B F2 N2 O'
_chemical_formula_weight         346.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-21 deposited with the CCDC.	2019-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                94.973(7)
_cell_angle_beta                 93.331(8)
_cell_angle_gamma                98.458(7)
_cell_formula_units_Z            2
_cell_length_a                   7.2247(7)
_cell_length_b                   8.2901(6)
_cell_length_c                   12.9787(14)
_cell_measurement_reflns_used    2006
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.0780
_cell_measurement_theta_min      2.4540
_cell_volume                     764.01(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_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    -83.00 -56.00   0.50    1.50    --    4.70  45.00 150.00   54
  2  \w    -46.00  39.00   0.50    1.50    --    4.70  45.00 150.00  170
  3  \w     42.00  94.00   0.50    1.50    --    4.70  45.00 150.00  104
  4  \w    -78.00  94.00   0.50    1.50    --    4.70  45.00  60.00  344
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0009968000
_diffrn_orient_matrix_UB_12      0.0040182000
_diffrn_orient_matrix_UB_13      0.0547749000
_diffrn_orient_matrix_UB_21      -0.0022564000
_diffrn_orient_matrix_UB_22      0.0854580000
_diffrn_orient_matrix_UB_23      0.0020052000
_diffrn_orient_matrix_UB_31      -0.0994836000
_diffrn_orient_matrix_UB_32      -0.0152750000
_diffrn_orient_matrix_UB_33      -0.0045504000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7323
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.495
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              FR-E+
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89934
_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            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: PhCl diff. Hex'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0722P)^2^+0.0786P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2131
_reflns_number_total             2772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9pp00410f2.cif
_cod_data_source_block           phen-py
_cod_original_cell_volume        764.01(12)
_cod_database_code               1552887
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H B F O'
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.973
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C4(H4), C6(H6), C9(H9), C17(H17), C19(H19), C8(H8), C7(H7), C3(H3),
 C14(H14), C12(H12), C18(H18), C13(H13)
;
_shelx_res_checksum              23337
_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 1.245
_oxdiff_exptl_absorpt_empirical_full_min 0.829