Synthesis of fulvene-containing boron complexes with aggregation-induced emission and mechanochromic luminescence.
Yan, Cai-Xin; Lin, Qian-Qian; Li, Sha; Wu, Cheng-Juan; Li, Yan-An; Fan, Jian-Zhong; Ma, Jian-Ping; Geng, Yan; Dong, Yu-Bin; Chemical communications (Cambridge, England) 56 (2020) 14435–14438; doi:10.1039/d0cc05757f

data_7127758
_publ_section_title
;
 Synthesis of fulvene-containing boron complexes with aggregation-induced
 emission and mechanochromic luminescence.
;
_journal_issue                   92
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              14435
_journal_page_last               14438
_journal_paper_doi               10.1039/d0cc05757f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C25 H25 B F2 O4'
_chemical_formula_sum            'C25 H25 B F2 O4'
_chemical_formula_weight         438.26
_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             2018-08-30
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2019-05-08 deposited with the CCDC.	2020-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                101.355(6)
_cell_angle_beta                 97.002(6)
_cell_angle_gamma                104.391(6)
_cell_formula_units_Z            2
_cell_length_a                   7.8130(6)
_cell_length_b                   9.3837(6)
_cell_length_c                   16.3462(11)
_cell_measurement_reflns_used    2430
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.6480
_cell_measurement_theta_min      10.3100
_cell_volume                     1119.53(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9784
_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  80.00   1.00    1.10    --   54.00 -37.00 -30.00   69
  2  \w     36.00 124.00   1.00    1.10    --   54.00  37.00   0.00   88
  3  \w    142.00 168.00   1.00    1.10    --  108.00  63.00 -60.00   26
  4  \w    117.00 142.00   1.00    1.10    --  108.00 -25.00 -60.00   25
  5  \w     93.00 127.00   1.00    1.10    --  108.00 -37.00 -60.00   34
  6  \w     88.00 114.00   1.00    1.10    --  108.00-111.00  30.00   26
  7  \w     65.00 113.00   1.00    1.10    --  108.00-111.00 -90.00   48
  8  \w     55.00  81.00   1.00    1.10    --   54.00-125.00-180.00   26
  9  \w     38.00 127.00   1.00    1.10    --  108.00 -50.00-180.00   89
 10  \w     51.00  79.00   1.00    1.10    --  108.00 -37.00 -60.00   28
 11  \w     38.00 131.00   1.00    1.10    --  108.00 -77.00 -60.00   93
 12  \w     44.00 111.00   1.00    1.10    --   54.00-125.00 -30.00   67
 13  \w     39.00 129.00   1.00    1.10    --  108.00 -50.00  60.00   90
 14  \w     88.00 155.00   1.00    1.10    --  108.00  63.00 -30.00   67
 15  \w     37.00 145.00   1.00    1.10    --  108.00 -91.00  90.00  108
 16  \w     36.00 175.00   1.00    1.10    --  108.00  12.00 -60.00  139
 17  \w     35.00  86.00   1.00    1.10    --  108.00 -25.00 -60.00   51
 18  \w     23.00  48.00   1.00    1.10    --   54.00 -57.00 -60.00   25
 19  \w     -2.00  30.00   1.00    1.00    --    0.00 -77.00-120.00   32
 20  \w    -10.00  80.00   1.00    1.10    --   54.00 -37.00-180.00   90
 21  \w     24.00  72.00   1.00    1.10    --   54.00-125.00-150.00   48
 22  \w    -69.00 -13.00   1.00    1.00    --    0.00 -77.00-120.00   56
 23  \w     25.00  70.00   1.00    1.00    --    0.00  77.00 -60.00   45
 24  \w     31.00 104.00   1.00    1.10    --   54.00  37.00 150.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1340833000
_diffrn_orient_matrix_UB_12      -0.1424427000
_diffrn_orient_matrix_UB_13      0.0116589000
_diffrn_orient_matrix_UB_21      0.1338124000
_diffrn_orient_matrix_UB_22      -0.0045540000
_diffrn_orient_matrix_UB_23      0.0762372000
_diffrn_orient_matrix_UB_31      -0.0833178000
_diffrn_orient_matrix_UB_32      0.1005777000
_diffrn_orient_matrix_UB_33      0.0600130000
_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  0.0190
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7135
_diffrn_reflns_theta_full        67.05
_diffrn_reflns_theta_max         67.05
_diffrn_reflns_theta_min         5.01
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.124
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0497P)^2^+0.2060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                3093
_reflns_number_total             4005
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0cc05757f2.cif
_cod_data_source_block           exp_2837
_cod_original_cell_volume        1119.52(13)
_cod_database_code               7127758
_chemical_oxdiff_formula         'C1 H1 N1 O1 B1 F1'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C12(H12), C16(H16), C17(H17),
 C19(H19), C20(H20)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.010
_oxdiff_exptl_absorpt_empirical_full_min 0.825