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_7246404
_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
_audit_creation_date             2023-02-27
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.19620(10)
_cell_length_b                   14.59640(10)
_cell_length_c                   15.1337(2)
_cell_measurement_reflns_used    8369
_cell_measurement_temperature    276.85(13)
_cell_measurement_theta_max      75.5580
_cell_measurement_theta_min      2.8930
_cell_volume                     2694.11(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      276.85(13)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9665
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.000
_diffrn_reflns_theta_min         4.208
_exptl_absorpt_coefficient_mu    2.188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41438
_exptl_absorpt_correction_type   none
_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          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 1650 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(8)
_refine_ls_extinction_coef       0.0092(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0605P)^2^+0.1610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.620
_reflns_Friedel_fraction_full    0.832
_reflns_Friedel_fraction_max     0.787
_reflns_number_gt                4464
_reflns_number_total             4738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01590k2.cif
_cod_data_source_block           na
_cod_depositor_comments
'Adding full bibliography for 7246404--7246410.cif.'
_cod_database_code               7246404
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.669
_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
 C25-C26B \\sim C25-C26A
 with sigma of 0.02
 C27B-C28 \\sim C27A-C28
 with sigma of 0.02
3. Rigid bond restraints
 C26B, C27B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Rigid body (RIGU) restrains
 B1, C29, C30, C25, C26B, C28, C27B, C32B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 B1, C25, C28, C29, C30, C26A, C27A, C32A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C26B)=Sof(H26B)=Sof(C27B)=Sof(H28A)=Sof(C32B)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=1-FVAR(1)
 Sof(H28)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=
 Sof(H32F)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C26B(H26B), C28(H28A), C28(H28), C19(H19), C17(H17), C11(H11), C1(H1),
 C12(H12), C5(H5), C13(H13), C2(H2), C4(H4), C3(H3), C26A(H26A)
6.b Fitted hexagon refined as free rotating group:
 C25(C26B,C27B,C28,C29,C30)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C33(H33A,H33B,H33C), C31(H31A,H31B,H31C), C23(H23A,H23B,
 H23C), C21(H21A,H21B,H21C), C32B(H32A,H32B,H32C), C32A(H32D,H32E,H32F)
;
_shelx_res_checksum              67603
_olex2_submission_special_instructions 'No special instructions were received'