Structural and mechanistic studies of excitation- and temperature-tunable multicolor luminescence of triarylborane
Xie, Yangbin; Dai, Songshan; Wang, Yue; Wang, Xi; Sun, Ying; Ju, Zhenghua; Fang, Ran; Zhang, Baoxin; Wu, Jincai; Zhang, Xiaoxiang; Pan, Xiaobo; CrystEngComm 25 (2023) 2204–2212; doi:10.1039/D2CE01590K

data_7246406
_publ_section_title
;
 Structural and mechanistic studies of excitation- and temperature-tunable
 multicolor luminescence of triarylborane
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2204
_journal_page_last               2212
_journal_paper_doi               10.1039/D2CE01590K
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C32 H30 B Br'
_chemical_formula_sum            'C32 H30 B Br'
_chemical_formula_weight         505.28
_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     iterative
_audit_creation_date             2023-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-01 deposited with the CCDC.	2023-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                71.759(3)
_cell_angle_beta                 81.597(4)
_cell_angle_gamma                81.225(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3292(5)
_cell_length_b                   12.1601(4)
_cell_length_c                   12.7627(5)
_cell_measurement_reflns_used    8672
_cell_measurement_temperature    298.78(10)
_cell_measurement_theta_max      75.7180
_cell_measurement_theta_min      3.6310
_cell_volume                     1351.51(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.78(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.924
_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     -9.00  19.00   1.00    0.10    --   44.07 -19.00 -30.00   28
  2  \w    -27.00   0.00   1.00    0.10    --   44.07 -19.00 -90.00   27
  3  \w    -15.00  22.00   1.00    0.10    --   44.07 -19.00-180.00   37
  4  \w     83.00 136.00   1.00    0.40    --  109.62 112.00 -87.00   53
  5  \w     99.00 169.00   1.00    0.40    --  109.62  61.00   0.00   70
  6  \w     65.00  95.00   1.00    0.40    --  109.62 -77.00-120.00   30
  7  \w     40.00  66.00   1.00    0.40    --  109.62 -61.00-150.00   26
  8  \w     41.00  66.00   1.00    0.40    --  109.62 -61.00   0.00   25
  9  \w     36.00  67.00   1.00    0.40    --  109.62 -61.00  30.00   31
 10  \w     37.00  68.00   1.00    0.40    --  109.62 -61.00  60.00   31
 11  \w     77.00 111.00   1.00    0.40    --  109.62-125.00  60.00   34
 12  \w     47.00 108.00   1.00    0.40    --  109.62-125.00   0.00   61
 13  \w     38.00  96.00   1.00    0.40    --  109.62 -94.00-150.00   58
 14  \w     50.00 107.00   1.00    0.40    --  109.62-112.00 179.00   57
 15  \w     11.00  71.00   1.00    0.10    --   44.07-112.00 179.00   60
 16  \w   -107.00 -29.00   1.00    0.40    -- -100.00 110.00  73.55   78
 17  \w   -123.00 -97.00   1.00    0.40    -- -100.00 141.00 112.62   26
 18  \w   -109.00 -46.00   1.00    0.40    -- -100.00 125.00  90.00   63
 19  \w    -71.00 -37.00   1.00    0.40    -- -100.00 141.00 112.62   34
 20  \w   -108.00 -55.00   1.00    0.40    -- -100.00 112.00 -87.00   53
 21  \w    -78.00 -52.00   1.00    0.10    --  -44.07 112.00 -87.00   26
 22  \w    -37.00  21.00   1.00    0.10    --  -44.07  37.00-180.00   58
 23  \w    -53.00 -26.00   1.00    0.40    -- -100.00  45.00-180.00   27
 24  \w    -62.00 -31.00   1.00    0.40    -- -100.00  61.00  30.00   31
 25  \w    -67.00 -37.00   1.00    0.40    -- -100.00  77.00  60.00   30
 26  \w   -103.00 -75.00   1.00    0.40    -- -100.00  77.00  60.00   28
 27  \w    -52.00 -27.00   1.00    0.40    -- -100.00  45.00 150.00   25
 28  \w    -54.00 -28.00   1.00    0.40    -- -100.00  45.00  90.00   26
 29  \w    -54.00 -29.00   1.00    0.40    -- -100.00  45.00-120.00   25
 30  \w   -176.00 -83.00   1.00    0.40    -- -100.00 -30.00-120.00   93
 31  \w   -169.00 -74.00   1.00    0.40    -- -100.00 -77.00-150.00   95
 32  \w   -140.00 -80.00   1.00    0.40    -- -100.00 -30.00 -90.00   60
 33  \w   -172.00-146.00   1.00    0.40    -- -100.00 -30.00 -90.00   26
 34  \w   -116.00 -25.00   1.00    0.10    --  -44.07 -57.00 -60.00   91
 35  \w   -114.00 -18.00   1.00    0.10    --  -44.07 -77.00  60.00   96
 36  \w   -167.00-139.00   1.00    0.40    -- -100.00 -45.00 150.00   28
 37  \w   -172.00-141.00   1.00    0.40    -- -100.00 -94.00 120.00   31
 38  \w   -135.00 -95.00   1.00    0.40    -- -100.00 -94.00 120.00   40
 39  \w   -120.00 -94.00   1.00    0.40    -- -100.00-112.00 179.00   26
 40  \w   -120.00 -64.00   1.00    0.10    --  -44.07-179.00-180.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1018326000
_diffrn_orient_matrix_UB_12      -0.0050237000
_diffrn_orient_matrix_UB_13      0.0865550000
_diffrn_orient_matrix_UB_21      -0.1299787000
_diffrn_orient_matrix_UB_22      -0.0160337000
_diffrn_orient_matrix_UB_23      0.0908850000
_diffrn_orient_matrix_UB_31      0.0310577000
_diffrn_orient_matrix_UB_32      -0.1332077000
_diffrn_orient_matrix_UB_33      0.0240984000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13296
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.944
_diffrn_reflns_theta_min         3.667
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0629P)^2^+0.4945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4540
_reflns_number_total             5212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01590k2.cif
_cod_data_source_block           xyb_0221_1-12_auto
_cod_depositor_comments
'Adding full bibliography for 7246404--7246410.cif.'
_cod_database_code               7246406
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.695
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C17(H17), C13(H13), C19(H19), C1(H1), C11(H11), C26(H26), C5(H5),
 C2(H2), C12(H12), C3(H3), C4(H4)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              14050
_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 2.205
_oxdiff_exptl_absorpt_empirical_full_min 0.310