Solvent-sensitive circularly polarized luminescent compounds bearing a 9,9'-spirobi[fluorene] skeleton.
Kubo, Masahiro; Takase, Ko; Noguchi, Keiichi; Nakano, Koji; Organic & biomolecular chemistry 18 (2020) 2866–2876; doi:10.1039/c9ob02681a

data_7157410
_publ_section_title
;
 Solvent-sensitive circularly polarized luminescent compounds bearing a
 9,9'-spirobi[fluorene] skeleton.
;
_journal_issue                   15
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2866
_journal_page_last               2876
_journal_paper_doi               10.1039/c9ob02681a
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         '2(C51 H32 N4), 2(C H4 O), C1 H2 Cl2'
_chemical_formula_sum            'C105 H74 Cl2 N8 O2'
_chemical_formula_weight         1550.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-12-13 deposited with the CCDC.	2020-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.7876(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.19377(18)
_cell_length_b                   39.0375(7)
_cell_length_c                   11.4370(2)
_cell_measurement_reflns_used    64729
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      68.19
_cell_measurement_theta_min      3.40
_cell_volume                     4062.81(13)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, 2004)'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      203(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            73644
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.216
_diffrn_reflns_theta_min         4.331
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 6047 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.126(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         14564
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1239P)^2^+1.0220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1809
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                13503
_reflns_number_total             14564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob02681a2.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 7157410.cif.'
_cod_original_cell_volume        4062.80(13)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7157410
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.871
_shelxl_version_number           2014-3
_shelx_res_checksum              84987
_shelx_hkl_checksum              92045