Axially Chiral Spiro-Conjugated Carbon-Bridged <i>p</i>-Phenylenevinylene Congeners: Synthetic Design and Materials Properties.
Hamada, Hiroyoshi; Itabashi, Yuki; Shang, Rui; Nakamura, Eiichi; Journal of the American Chemical Society 142 (2020) 2059–2067; doi:10.1021/jacs.9b13019

data_4133981
_publ_section_title
;
 Axially Chiral Spiro-Conjugated Carbon-Bridged <i>p</i>-Phenylenevinylene
 Congeners: Synthetic Design and Materials Properties.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2059
_journal_page_last               2067
_journal_paper_doi               10.1021/jacs.9b13019
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C55 H36, 2(C H2 Cl2)'
_chemical_formula_sum            'C57 H40 Cl4'
_chemical_formula_weight         866.69
_chemical_name_common            spiroCC
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.900(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9001(3)
_cell_length_b                   15.8666(4)
_cell_length_c                   22.7472(5)
_cell_measurement_reflns_used    19630
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      3.99
_cell_volume                     4186.6(2)
_computing_cell_refinement       'Rapid Auto (Rigaku)'
_computing_data_collection       'Rapid Auto (Rigaku)'
_computing_data_reduction        'Rapid Auto (Rigaku)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23863
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         3.987
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.877
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7327
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0402P)^2^+3.9863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3230
_reflns_number_total             3828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13019_si_002.cif
_cod_data_source_block           spiro_a
_cod_depositor_comments          'Adding full bibliography for 4133981.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4133981
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.730
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              45427
_shelx_hkl_checksum              96414