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_7246409
_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      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             2023-02-27
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-03-01 deposited with the CCDC.	2023-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.18719(19)
_cell_length_b                   14.6021(2)
_cell_length_c                   15.1221(2)
_cell_measurement_reflns_used    7952
_cell_measurement_temperature    299.50(18)
_cell_measurement_theta_max      76.1200
_cell_measurement_theta_min      4.1840
_cell_volume                     2691.11(7)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.50(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_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     40.00  68.00   0.50    0.07    --  109.62 -61.00  60.00   56
  2  \w     50.00 108.00   0.50    0.07    --  109.62-125.00   0.00  116
  3  \w     41.00 107.00   0.50    0.07    --  109.62-106.00 -82.00  132
  4  \w     36.00  61.00   0.50    0.07    --  109.62 -61.00   0.00   50
  5  \w     90.00 175.00   0.50    0.07    --  109.62  24.00 -91.00  170
  6  \w     79.00 116.00   0.50    0.05    --   44.32 179.00  60.00   74
  7  \w     -9.00  32.00   0.50    0.05    --  -44.32  24.00 -91.00   82
  8  \w    -56.00 -28.00   0.50    0.07    -- -100.00  61.00-180.00   56
  9  \w    -54.00 -27.00   0.50    0.07    -- -100.00  45.00-180.00   54
 10  \w    -50.00 -25.00   0.50    0.07    -- -100.00  45.00 -30.00   50
 11  \w    -29.00  25.00   0.50    0.05    --  -44.32  19.00  30.00  108
 12  \w    -29.00  33.00   0.50    0.05    --  -44.32  19.00 150.00  124
 13  \w    -54.00 -29.00   0.50    0.07    -- -100.00  45.00  60.00   50
 14  \w    -83.00 -56.00   0.50    0.07    -- -100.00 112.00 106.00   54
;
_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      -0.0394849000
_diffrn_orient_matrix_UB_12      0.0861568000
_diffrn_orient_matrix_UB_13      -0.0494322000
_diffrn_orient_matrix_UB_21      -0.0045843000
_diffrn_orient_matrix_UB_22      -0.0550596000
_diffrn_orient_matrix_UB_23      -0.0868214000
_diffrn_orient_matrix_UB_31      -0.1200044000
_diffrn_orient_matrix_UB_32      -0.0262365000
_diffrn_orient_matrix_UB_33      0.0196064000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9650
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.319
_diffrn_reflns_theta_min         4.209
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.191
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58609
_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    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 1679 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.015(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4881
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0681P)^2^+0.0786P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1039
_reflns_Friedel_coverage         0.610
_reflns_Friedel_fraction_full    0.829
_reflns_Friedel_fraction_max     0.749
_reflns_number_gt                4572
_reflns_number_total             4881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01590k2.cif
_cod_data_source_block           xyb_0222-1_auto
_cod_depositor_comments
'Adding full bibliography for 7246404--7246410.cif.'
_cod_database_code               7246409
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.957
_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. Rigid body (RIGU) restrains
 C19, C18, C17, C16, C15, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C1(H1), C5(H5), C26(H26), C12(H12), C11(H11), C28(H28), C2(H2),
 C13(H13), C4(H4), C17(H17), C3(H3)
3.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C22(H22A,H22B,
 H22C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              21983
_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 1.821
_oxdiff_exptl_absorpt_empirical_full_min 0.585