Facile synthesis, aggregation-induced emission, mechano- and thermochromism of o-carborane–tetraphenylethene dyads with a short CH(OH) linker
Li, Tianrui; Zhang, Hao; Miao, Jinling; Xu, Chunyue; Nie, Yong; Liu, Guangning; Sun, Guoxin; Jiang, Xuchuan; New Journal of Chemistry 47 (2023) 18243–18250; doi:10.1039/D3NJ03431C

data_7062695
_publ_section_title
;
 Facile synthesis, aggregation-induced emission, mechano- and
 thermochromism of o-carborane--tetraphenylethene dyads with a short
 CH(OH) linker
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18243
_journal_page_last               18250
_journal_paper_doi               10.1039/D3NJ03431C
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C29 H32 B10 O0.98'
_chemical_formula_sum            'C29 H32 B10 O0.97'
_chemical_formula_weight         504.25
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-03-07 deposited with the CCDC.	2023-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                78.019(6)
_cell_angle_beta                 88.318(6)
_cell_angle_gamma                69.186(7)
_cell_formula_units_Z            2
_cell_length_a                   9.9704(8)
_cell_length_b                   11.7142(7)
_cell_length_c                   13.6657(10)
_cell_measurement_reflns_used    4845
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4080
_cell_measurement_theta_min      3.5910
_cell_volume                     1457.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -11.00  84.00   1.00    3.19    --   16.01  77.00-120.00   95
  2  \w    -52.00  43.00   1.00    3.19    --   16.01 -77.00 120.00   95
  3  \w     -1.00  83.00   1.00    3.19    --   16.01  57.00  90.00   84
  4  \w    -53.00  35.00   1.00    3.19    --   16.01 -37.00 -30.00   88
  5  \w    -25.00  22.00   1.00    3.19    --  -17.11 -99.00 -90.00   47
  6  \w    -25.00  55.00   1.00    3.19    --   16.01 -99.00 -60.00   80
  7  \w     -3.00  61.00   1.00    3.19    --   16.01  37.00  30.00   64
  8  \w     35.00  88.00   1.00    3.19    --   16.01 178.00 -30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0628780000
_diffrn_orient_matrix_UB_12      0.0149304000
_diffrn_orient_matrix_UB_13      -0.0089457000
_diffrn_orient_matrix_UB_21      -0.0381497000
_diffrn_orient_matrix_UB_22      0.0613093000
_diffrn_orient_matrix_UB_23      0.0071921000
_diffrn_orient_matrix_UB_31      0.0199247000
_diffrn_orient_matrix_UB_32      -0.0202482000
_diffrn_orient_matrix_UB_33      0.0518673000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17889
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
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    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+0.3481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                4173
_reflns_number_total             5943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3nj03431c2.cif
_cod_data_source_block           180417_ny_zh_52_b
_cod_depositor_comments
'Adding full bibliography for 7062695--7062696.cif.'
_cod_original_cell_volume        1457.70(18)
_cod_database_code               7062695
_chemical_oxdiff_formula         'C H B O'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1, B1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C1, B4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C2, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 B2, B3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 B4, B9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H0AA(0.5) H1B(0.5)
4.a Ternary CH refined with riding coordinates:
 C3(H3A), C3(H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C7(H7), C8(H8), C6(H6), C5(H5), C21(H21), C25(H25), C22(H22),
 C27(H27), C23(H23), C20(H20), C26(H26), C15(H15), C16(H16), C29(H29), C13(H13),
  C28(H28), C17(H17), C14(H14)
4.c Tetrahedral OH refined with riding coordinates:
 O1(H1B)
4.d Idealised tetrahedral OH refined as rotating group:
 O0AA(H0AA)
4.e Boron cage BH refined with riding coordinates:
 B5(H5A), B1(H1), B10(H10), C1(H1A), B9(H9), B6(H6A), B4(H4), B8(H8A), B7(H7A),
  B2(H2), B3(H3)
;
_olex2_date_sample_data_collection 2018-04-17
_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 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.853