Synthesis of Selectively 4-Substituted 9,9´-Spirobifluorenes and Modulation of Their Photophysical Properties.
Kaiser, Reinhard Peter; Mosinger, Jiri; Cisarova, Ivana; Kotora, Martin; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB01319A

data_7155699
_publ_section_title
;
 Synthesis of Selectively 4-Substituted 9,9&#x00B4;-Spirobifluorenes and
 Modulation of Their Photophysical Properties.
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB01319A
_journal_year                    2017
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C46 H38'
_chemical_formula_sum            'C46 H38'
_chemical_formula_weight         590.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-04 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8419(5)
_cell_length_b                   8.6097(2)
_cell_length_c                   23.3066(6)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      69.8489
_cell_measurement_theta_min      3.8399
_cell_volume                     3338.49(15)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service v4.2.9'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios Cu  multilayer optic'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25788
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.248
_diffrn_reflns_theta_min         3.840
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.9813
_exptl_absorpt_correction_T_min  0.8991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       bar
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+2.5170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5047
_reflns_number_total             6307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ob01319a2.cif
_cod_data_source_block           cu_rk_384_kotora
_cod_database_code               7155699
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              4916