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_7246408
_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                   12.19550(10)
_cell_length_b                   14.59670(10)
_cell_length_c                   15.13390(10)
_cell_measurement_reflns_used    8280
_cell_measurement_temperature    276.17(13)
_cell_measurement_theta_max      75.5170
_cell_measurement_theta_min      3.0310
_cell_volume                     2694.05(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      276.17(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.946
_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     45.00  90.00   0.50    0.05    --  109.26 -76.00  13.00   90
  2  \w     78.00 103.00   0.50    0.05    --  109.26 -77.00  30.00   50
  3  \w     35.00  67.00   0.50    0.05    --  109.26 -61.00  60.00   64
  4  \w     57.00 100.00   0.50    0.05    --  109.26 -77.00 150.00   86
  5  \w     35.00  61.00   0.50    0.05    --  109.26 -61.00 150.00   52
  6  \w     21.00 104.00   0.50    0.05    --   43.05  45.00 -11.00  166
  7  \w    112.00 174.00   0.50    0.05    --  109.26  76.00 140.00  124
  8  \w    -36.00   7.00   0.50    0.05    --   43.05 -19.00  30.00   86
  9  \w   -116.00 -67.00   0.50    0.05    --  -43.05-179.00  60.00   98
 10  \w    -54.00 -29.00   0.50    0.05    -- -100.00  45.00 -11.00   50
 11  \w    -49.00 -24.00   0.50    0.05    -- -100.00  45.00   0.00   50
 12  \w    -52.00 -24.00   0.50    0.05    -- -100.00  45.00 -30.00   56
 13  \w    -54.00 -29.00   0.50    0.05    -- -100.00  45.00 -90.00   50
 14  \w   -102.00 -30.00   0.50    0.05    -- -100.00 118.00-144.00  144
 15  \w    -53.00 -25.00   0.50    0.05    -- -100.00  45.00  90.00   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      0.0044853000
_diffrn_orient_matrix_UB_12      -0.1036569000
_diffrn_orient_matrix_UB_13      0.0188993000
_diffrn_orient_matrix_UB_21      -0.0715263000
_diffrn_orient_matrix_UB_22      0.0140624000
_diffrn_orient_matrix_UB_23      0.0827757000
_diffrn_orient_matrix_UB_31      -0.1040144000
_diffrn_orient_matrix_UB_32      -0.0141538000
_diffrn_orient_matrix_UB_33      -0.0561357000
_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  0.0267
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9835
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.788
_diffrn_reflns_theta_min         4.208
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 1598 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.012(9)
_refine_ls_extinction_coef       0.0109(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4703
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+0.2458P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.578
_reflns_Friedel_fraction_full    0.782
_reflns_Friedel_fraction_max     0.701
_reflns_number_gt                4461
_reflns_number_total             4703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01590k2.cif
_cod_data_source_block           xieyb_0331_300k
_cod_depositor_comments
'Adding full bibliography for 7246404--7246410.cif.'
_cod_database_code               7246408
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.749
_shelx_estimated_absorpt_t_min   0.611
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C27B-C26 \\sim C27A-C26
 with sigma of 0.02
 C29-C28A \\sim C28B-C29
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C28B, C31B, C27A, C26, C25, C24, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C27B, C31A, C28A, C26, C25, C24, C29
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Others
 Sof(H26A)=Sof(C27B)=Sof(C28A)=Sof(H28A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=1-FVAR(1)
 Sof(H26)=Sof(C28B)=Sof(H28B)=Sof(C27A)=Sof(C31B)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C13(H13), C17(H17), C26(H26A), C26(H26), C28A(H28A), C5(H5),
 C12(H12), C1(H1), C11(H11), C2(H2), C4(H4), C3(H3), C28B(H28B)
5.b Fitted hexagon refined as free rotating group:
 C25(C26,C27B,C28A,C29,C24)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C23(H23A,H23B,H23C), C30(H30A,H30B,
 H30C), C22(H22A,H22B,H22C), C31A(H31A,H31B,H31C), C31B(H31D,H31E,H31F)
;
_shelx_res_checksum              84841
_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 1.480
_oxdiff_exptl_absorpt_empirical_full_min 0.628