AIEE-active V-shaped fused-biscoumarins: synthesis, photophysical and electroluminescence properties
Li, Debao; Li, Peiying; Zhao, Yuling; Su, Ruige; Guo, Yongchun; Su, Wenming; Yu, Tianzhi; New Journal of Chemistry 46 (2022) 23213–23224; doi:10.1039/D2NJ03977J

data_7062095
_publ_section_title
;
 AIEE-active V-shaped fused-biscoumarins: synthesis, photophysical and
 electroluminescence properties
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              23213
_journal_page_last               23224
_journal_paper_doi               10.1039/D2NJ03977J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C40 H31 N O4'
_chemical_formula_sum            'C40 H31 N O4'
_chemical_formula_weight         589.66
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-10 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                78.317(5)
_cell_angle_beta                 72.954(6)
_cell_angle_gamma                67.296(5)
_cell_formula_units_Z            4
_cell_length_a                   12.7991(8)
_cell_length_b                   16.2884(9)
_cell_length_c                   16.7129(11)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.2240
_cell_measurement_theta_min      2.9450
_cell_volume                     3057.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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    -66.00  33.00   1.00    1.00    --  -41.11  38.00 -30.00   99
  2  \w    -61.00  32.00   1.00    1.00    --  -41.11  57.00-180.00   93
  3  \w     25.00  52.00   1.00    1.00    --   41.11-125.00-120.00   27
  4  \w     58.00  92.00   1.00    1.00    --   41.11-125.00 -30.00   34
  5  \w     88.00 121.00   1.00    2.00    --  106.95-125.00-120.00   33
  6  \w     37.00 116.00   1.00    2.00    --  106.95-125.00  30.00   79
  7  \w     79.00 139.00   1.00    2.00    --  106.95 -77.00  90.00   60
  8  \w     73.00 115.00   1.00    2.00    --  106.95-125.00  90.00   42
  9  \w     54.00 135.00   1.00    2.00    --  106.95 -61.00 150.00   81
 10  \w     86.00 160.00   1.00    2.00    --  106.95  61.00 120.00   74
 11  \w    118.00 166.00   1.00    2.00    --  106.95 125.00  30.00   48
 12  \w    108.00 153.00   1.00    2.00    --  106.95 125.00 150.00   45
 13  \w     94.00 177.00   1.00    2.00    --  106.95 125.00  60.00   83
 14  \w     79.00 173.00   1.00    2.00    --  106.95  30.00-120.00   94
 15  \w    109.00 169.00   1.00    2.00    --  106.95 125.00-180.00   60
 16  \w     36.00  98.00   1.00    2.00    --  106.95 -61.00  60.00   62
 17  \w     78.00 172.00   1.00    2.00    --  106.95  77.00 150.00   94
 18  \w   -108.00 -15.00   1.00    1.00    --  -41.11 -57.00  30.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1070313000
_diffrn_orient_matrix_UB_12      -0.0237485000
_diffrn_orient_matrix_UB_13      0.0532626000
_diffrn_orient_matrix_UB_21      0.0148110000
_diffrn_orient_matrix_UB_22      0.0252799000
_diffrn_orient_matrix_UB_23      0.0789469000
_diffrn_orient_matrix_UB_31      -0.0798162000
_diffrn_orient_matrix_UB_32      0.0970425000
_diffrn_orient_matrix_UB_33      -0.0179585000
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22589
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.736
_diffrn_reflns_theta_min         2.780
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         11987
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0835P)^2^+0.5286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9726
_reflns_number_total             11987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03977j1.cif
_cod_data_source_block           10633-2
_cod_depositor_comments
'Adding full bibliography for 7062095--7062096.cif.'
_cod_original_cell_volume        3057.2(3)
_cod_database_code               7062095
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.914
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C012-H012
 0.8 with sigma of 0.01
 C43-H43
 0.85 with sigma of 0.01
 C12-H12
 0.85 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C38(H38A,H38B), C77(H77A,H77B), C79(H79A,H79B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C012(H012), C13(H13), C15(H15), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C42(H42), C46(H46), C53(H53),
 C54(H54), C55(H55), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C66(H66),
  C67(H67), C68(H68), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74),
 C75(H75), C76(H76)
3.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C78(H78A,H78B,H78C), C80(H80A,H80B,
 H80C)
;
_shelx_res_checksum              58122
_olex2_date_sample_data_collection 2021-12-29
_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 1.956
_oxdiff_exptl_absorpt_empirical_full_min 0.398