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_7127759
_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         'C31 H26 O2'
_chemical_formula_sum            'C31 H26 O2'
_chemical_formula_weight         430.52
_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             2019-03-28
_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                75.480(5)
_cell_angle_beta                 73.810(6)
_cell_angle_gamma                83.749(6)
_cell_formula_units_Z            2
_cell_length_a                   9.6358(7)
_cell_length_b                   10.2626(6)
_cell_length_c                   12.5875(8)
_cell_measurement_reflns_used    3338
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.9460
_cell_measurement_theta_min      7.9690
_cell_volume                     1156.19(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
;
XL, 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 0.9942
_diffrn_measured_fraction_theta_max 0.9657
_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  39.00   1.00    1.00    --    0.00 -19.00 -30.00   28
  2  \w     28.00 122.00   1.00    1.00    --   54.00  37.00  30.00   94
  3  \w     79.00 157.00   1.00    1.00    --  108.00  77.00 -60.00   78
  4  \w    130.00 177.00   1.00    1.00    --  108.00  37.00 -90.00   47
  5  \w     99.00 129.00   1.00    1.00    --  108.00 -50.00 -60.00   30
  6  \w     90.00 116.00   1.00    1.00    --  108.00-111.00 -90.00   26
  7  \w     58.00 107.00   1.00    1.00    --   54.00-125.00-120.00   49
  8  \w     61.00  96.00   1.00    1.00    --  108.00 -50.00 -60.00   35
  9  \w     59.00 128.00   1.00    1.00    --  108.00 -77.00-120.00   69
 10  \w     43.00 128.00   1.00    1.00    --  108.00 -50.00  30.00   85
 11  \w     63.00 113.00   1.00    1.00    --  108.00 -77.00  60.00   50
 12  \w     35.00  85.00   1.00    1.00    --   54.00-125.00  90.00   50
 13  \w     36.00 112.00   1.00    1.00    --  108.00-111.00  60.00   76
 14  \w     36.00 134.00   1.00    1.00    --  108.00   0.00 120.00   98
 15  \w     79.00 169.00   1.00    1.00    --  108.00  77.00 -30.00   90
 16  \w     96.00 121.00   1.00    1.00    --   54.00  57.00 -90.00   25
 17  \w     90.00 123.00   1.00    1.00    --  108.00  37.00 -90.00   33
 18  \w     41.00 125.00   1.00    1.00    --  108.00 -50.00-180.00   84
 19  \w     40.00 108.00   1.00    1.00    --  108.00-111.00-150.00   68
 20  \w    -15.00  35.00   1.00    1.00    --   54.00 -77.00  90.00   50
 21  \w    -15.00  74.00   1.00    1.00    --   54.00 -57.00 120.00   89
 22  \w     43.00  69.00   1.00    1.00    --    0.00  57.00 150.00   26
 23  \w      0.00  33.00   1.00    1.00    --    0.00  57.00 150.00   33
 24  \w    -60.00  -8.00   1.00    1.00    --    0.00 -19.00 -30.00   52
 25  \w    -15.00  76.00   1.00    1.00    --   54.00 -37.00-150.00   91
;
_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      0.1445368000
_diffrn_orient_matrix_UB_12      -0.0790259000
_diffrn_orient_matrix_UB_13      0.0041194000
_diffrn_orient_matrix_UB_21      -0.0116572000
_diffrn_orient_matrix_UB_22      -0.0649675000
_diffrn_orient_matrix_UB_23      -0.0948634000
_diffrn_orient_matrix_UB_31      0.0820842000
_diffrn_orient_matrix_UB_32      0.1167140000
_diffrn_orient_matrix_UB_33      -0.0902198000
_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  0.0202
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7623
_diffrn_reflns_theta_full        71.26
_diffrn_reflns_theta_max         71.26
_diffrn_reflns_theta_min         3.76
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50900
_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            yellow
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0567P)^2^+0.4796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                3498
_reflns_number_total             4339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0cc05757f2.cif
_cod_data_source_block           exp_3232
_cod_original_cell_volume        1156.20(13)
_cod_database_code               7127759
_chemical_oxdiff_formula         'C1 H1 O1 N1'
_reflns_odcompleteness_completeness 99.42
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C23(H23), C13(H13), C19(H19), C30(H30), C31(H31), C1(H1A), C25(H25),
 C4(H4), C9(H9), C10(H10), C28(H28), C2(H2), C26(H26), C27(H27), C3(H3)
2.b Tetrahedral OH refined with riding coordinates:
 O1(H1)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.620