Halogen-containing bridged carborane–tetraphenylethene compounds: efficient and wide-range shifted excitation-dependent emissions
Li, Fengjiao; Dong, Yiran; Miao, Jinling; Nie, Yong; Zhang, Yujian; Li, Tianrui; Xu, Chunyue; Liu, Guangning; Jiang, Xuchuan; New Journal of Chemistry 48 (2024) 15532–15539; doi:10.1039/D4NJ02867H

data_7063394
_publ_section_title
;
 Halogen-containing bridged carborane--tetraphenylethene compounds:
 efficient and wide-range shifted excitation-dependent emissions
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15532
_journal_page_last               15539
_journal_paper_doi               10.1039/D4NJ02867H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C29 H30 B10 Cl F'
_chemical_formula_sum            'C29 H30 B10 Cl F'
_chemical_formula_weight         541.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-10-27 deposited with the CCDC.	2024-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.367(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1612(4)
_cell_length_b                   12.8676(4)
_cell_length_c                   31.9346(10)
_cell_measurement_reflns_used    12803
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.1240
_cell_measurement_theta_min      2.1320
_cell_volume                     5757.2(3)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -37.00  94.00   1.00    6.00    --    5.00  54.00 -36.00  131
  2  \w    -84.00  47.00   1.00    6.00    --    5.00 -54.00 179.00  131
  3  \w   -113.00  19.00   1.00    6.00    --  -23.80 -54.00 179.00  132
  4  \w    -66.00  66.00   1.00    6.00    --  -23.80  54.00 -36.00  132
  5  \w    -66.00  66.00   1.00    6.00    --  -23.80  57.00  60.00  132
  6  \w   -113.00  61.00   1.00    6.00    --  -23.80  19.00   0.00  174
  7  \w    -63.00 -37.00   1.00    6.00    --  -23.80  57.00-180.00   26
  8  \w     -3.00  24.00   1.00    6.00    --  -23.80  57.00-180.00   27
  9  \w   -113.00  14.00   1.00    6.00    --  -23.80 -70.00  90.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0098192000
_diffrn_orient_matrix_UB_12      0.0114933000
_diffrn_orient_matrix_UB_13      -0.0206511000
_diffrn_orient_matrix_UB_21      -0.0397037000
_diffrn_orient_matrix_UB_22      0.0341437000
_diffrn_orient_matrix_UB_23      -0.0030758000
_diffrn_orient_matrix_UB_31      0.0298645000
_diffrn_orient_matrix_UB_32      0.0417320000
_diffrn_orient_matrix_UB_33      0.0082168000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            8724
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.149
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59599
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         8724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+8.9826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2028
_refine_ls_wR_factor_ref         0.2076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7885
_reflns_number_total             8724
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9908\% 
 around [0.95 0.00 -0.31] (reciprocal) or [1.00 0.00 0.00] (direct)
;
_cod_data_source_file            d4nj02867h2.cif
_cod_data_source_block           r20231016b_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 7063394.cif.'
_cod_database_code               7063394
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.41(7)
 0.31(2) 0.14(5) 0.14(5)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Ternary CH refined with riding coordinates:
 C27(H27)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C26(H26)
3.c Boron cage BH refined with riding coordinates:
 C29(H29), B1(H1), B2(H2A), B3(H3A), B4(H4A), B5(H5A), B6(H6A), B7(H7), B8(H8),
  B9(H9A), B10(H10A)
;
_shelx_res_checksum              59803
_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 2.040
_oxdiff_exptl_absorpt_empirical_full_min 0.565
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2